A full set of iridium(iv) pyridine-alkoxide stereoisomers: highly geometry-dependent redox properties.
Shopov, Dimitar Y.; Rudshteyn, Benjamin; Campos, Jesús; Vinyard, David J.; Batista, Victor S.; Brudvig, Gary W.; Crabtree, Robert H.; Chemical science 8 (2017) 1642–1652; doi:10.1039/c6sc03758e

data_1544517
_publ_section_title
;
 A full set of iridium(iv) pyridine-alkoxide stereoisomers: highly
 geometry-dependent redox properties.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              1642
_journal_page_last               1652
_journal_paper_doi               10.1039/c6sc03758e
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         '2(C16 H20 Cl2 Ir N2 O2), C H2 Cl2'
_chemical_formula_sum            'C33 H42 Cl6 Ir2 N4 O4'
_chemical_formula_weight         1155.80
_chemical_name_common            'Ir(pyalk)2Cl2, "yellow isomer"'
_chemical_name_systematic
'cis-Cl, trans-O, cis-N-bis(2-{pyridin-2-yl}propan-2-olato)-dichloro-iridium(IV)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-08-03 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9782(4)
_cell_length_b                   15.0278(3)
_cell_length_c                   17.4463(12)
_cell_measurement_reflns_used    68335
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.023
_cell_volume                     3927.0(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            119682
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.220
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       Block
_exptl_crystal_F_000             2224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.948
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4503
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+21.1695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3872
_reflns_number_total             4503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc03758e2.cif
_cod_data_source_block           5iv
_cod_depositor_comments
;Adding full bibliography for 1544510--1544517.cif.

 Adding full bibliography for 1544510--1544517.cif.
;
_cod_database_code               1544517
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.326
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl3(0.5) C50(0.5) H50A(0.5) H50B(0.5) Cl4(0.5)
 Fixed Uiso: H1(0.034) H3(0.051) H12(0.044) H9(0.033) H4(0.052) H10(0.044)
 H2(0.042) H11(0.048) H16A(0.053) H16B(0.053) H16C(0.053) H15A(0.058)
 H15B(0.058) H15C(0.058) H7A(0.068) H7B(0.068) H7C(0.068) H8A(0.074) H8B(0.074)
 H8C(0.074) H50A(0.131) H50B(0.131)
 Fixed X: H1(-0.046) H3(0.0635) H12(-0.2538) H9(0.0136) H4(0.1611) H10(-
 0.1114) H2(-0.0413) H11(-0.247) H16A(-0.1898) H16B(-0.1261) H16C(-0.0842)
 H15A(-0.1904) H15B(-0.19) H15C(-0.2544) H7A(0.1108) H7B(0.2082) H7C(0.1975)
 H8A(0.2927) H8B(0.308) H8C(0.2699) H50A(0.0146) H50B(-0.0578)
 Fixed Y: H1(0.0834) H3(0.2361) H12(0.1705) H9(0.3193) H4(0.2951) H10(0.3998)
 H2(0.1288) H11(0.3232) H16A(0.0131) H16B(-0.0609) H16C(0.0184) H15A(0.0728)
 H15B(-0.0276) H15C(0.0445) H7A(0.3782) H7B(0.3786) H7C(0.3819) H8A(0.2446)
 H8B(0.2435) H8C(0.157) H50A(0.4054) H50B(0.4771)
 Fixed Z: H1(0.5016) H3(0.6655) H12(0.2765) H9(0.3115) H4(0.5748) H10(0.2732)
 H2(0.6283) H11(0.2551) H16A(0.234) H16B(0.2707) H16C(0.2212) H15A(0.4331)
 H15B(0.4025) H15C(0.3638) H7A(0.4124) H7B(0.3746) H7C(0.4658) H8A(0.4824)
 H8B(0.3916) H8C(0.4339) H50A(0.5607) H50B(0.5846)
;
_shelx_res_checksum              51883
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'