#======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _audit_creation_method 'Jana2006 Version : 19/10/2017' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C19 H34 N3 O2 P2 Re, C6 H6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C25 H40 N3 O2 P2 Re1' _chemical_formula_weight 662.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2xab;2ybc;2zac' _symmetry_Int_Tables_number 19 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z+1/2 4 x+1/2,-y+1/2,-z _cell_length_a 10.1881(7) _cell_length_b 13.7426(11) _cell_length_c 20.6392(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2889.7(4) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.990(15) 1 0 0 0 1 0 0 0 1 2 0.010(15) -1 0 0 0 -1 0 0 0 -1 _cell_formula_units_Z 4 _cell_measurement_reflns_used 1967 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 25.94 _cell_measurement_temperature 100 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.5234 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 4.34 _exptl_crystal_description needle _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.84 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 11512 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.3 _diffrn_reflns_theta_full 27.3 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_unetI/netI 0.1079 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 6403 _reflns_number_gt 4528 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_gt 0.0991 _refine_ls_R_factor_all 0.0764 _refine_ls_wR_factor_ref 0.1115 _refine_ls_goodness_of_fit_ref 1.11 _refine_ls_goodness_of_fit_gt 1.18 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 6403 _refine_ls_number_parameters 309 _refine_ls_number_restraints 2 _refine_ls_number_constraints 150 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0004I^2^)' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_shift/su_max 0.0360 _refine_ls_shift/su_mean 0.0014 _refine_diff_density_max 2.27 _refine_diff_density_min -1.10 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; 2792 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0.010(15) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Re -1.0185 7.2310 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection 'Apex 3 (Bruker, 2016)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2016)' _computing_data_reduction 'SAINT-Plus (Bruker, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _computing_structure_refinement 'Jana 2006 (Pet\