Solvent-Dependent Thermochemistry of an Iridium/Ruthenium H<sub>2</sub> Evolution Catalyst.
Brereton, Kelsey R.; Pitman, Catherine L.; Cundari, Thomas R.; Miller, Alexander J. M.; Inorganic chemistry 55 (2016) 12042–12051; doi:10.1021/acs.inorgchem.6b02223

data_4349271
_publ_section_title
;
 Solvent-Dependent Thermochemistry of an Iridium/Ruthenium H<sub>2</sub>
 Evolution Catalyst.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12042
_journal_page_last               12051
_journal_paper_doi               10.1021/acs.inorgchem.6b02223
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'2(C38 H37 Ir N8 Ru), 4(C F3 O3 S), C4 H10 O, 2(C2 H3 N)'
_chemical_formula_sum            'C88 H90 F12 Ir2 N18 O13 Ru2 S4'
_chemical_formula_weight         2550.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.633(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0146(7)
_cell_length_b                   20.9174(8)
_cell_length_c                   23.3149(9)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      2.88
_cell_volume                     9485.9(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            101444
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.191
_diffrn_reflns_theta_min         2.271
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.475
_exptl_absorpt_correction_T_max  0.8229
_exptl_absorpt_correction_T_min  0.3267
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0679 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.3970.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             5048
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.226
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         17696
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0723P)^2^+36.9961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13222
_reflns_number_total             17696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02223_si_002.cif
_cod_data_source_block           x1505014
_cod_database_code               4349271
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 S129, O130, O131, O132, C133, F134, F135, F136, S113, O114, O115, O116, C117,
 F118, F119, F120
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O143, C144, C145, C146, C147
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S121, O122, O123, O124, C125, F126, F127, F128, S129, O130, O131, O132, C133,
 F134, F135, F136
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(S121)=Sof(O122)=Sof(O123)=Sof(O124)=Sof(C125)=Sof(F126)=Sof(F127)=
 Sof(F128)=1-FVAR(1)
 Sof(S129)=Sof(O130)=Sof(O131)=Sof(O132)=Sof(C133)=Sof(F134)=Sof(F135)=
 Sof(F136)=FVAR(1)
4.a Free rotating group:
 S121(O122,O123,O124,C125,F126,F127,F128), S129(O130,O131,O132,C133,F134,F135,
 F136), S113(O114,O115,O116,C117,F118,F119,F120), O143(C144,C145,C146,C147,N140,
 C141,C142,N137,C138,C139)
4.b Secondary CH2 refined with riding coordinates:
 C144(H14A,H14B), C146(H14F,H14G)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C40(H40), C41(H41),
  C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C66(H66),
  C67(H67), C68(H68), C82(H82), C83(H83), C84(H84), C88(H88), C89(H89),
 C90(H90), C91(H91), C93(H93), C94(H94), C95(H95), C96(H96)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C145(H14C,H14D,H14E),
 C147(H14H,H14I,H14J), C142(H14K,H14L,H14M), C139(H13A,H13B,H13C)
;
_shelx_res_checksum              43266
_shelx_hkl_checksum              7150
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'