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_4349270
_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         'C40 H40 Ir N9 Ru, 4(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C46 H43 F12 Ir N10 O12 Ru S4'
_chemical_formula_weight         1577.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                91.6565(12)
_cell_angle_beta                 103.3523(11)
_cell_angle_gamma                119.0556(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8260(3)
_cell_length_b                   15.0728(3)
_cell_length_c                   17.1738(4)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.567
_cell_measurement_theta_min      2.682
_cell_volume                     3218.93(13)
_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      100.15
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35171
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         2.681
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.909
_exptl_absorpt_correction_T_max  0.6758
_exptl_absorpt_correction_T_min  0.2359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0762 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.3491.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       plate
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         11013
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0502P)^2^+9.0378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10115
_reflns_number_total             11013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02223_si_002.cif
_cod_data_source_block           x1603010
_cod_original_cell_volume        3218.93(12)
_cod_database_code               4349270
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.184
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 S103, C96, O97, O98, O99, F100, F101, F102, S8AA, C96A, O97A, O98A, O104, F1,
 F2, F105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S76, C80, O77, O78, O79, F81, F82, F83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, C69, O70, O71, O72, F73, F74, F75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(S8AA)=Sof(C96A)=Sof(O97A)=Sof(O98A)=Sof(O104)=Sof(F1)=Sof(F2)=Sof(F105)=1-
 FVAR(1)
 Sof(S103)=Sof(C96)=Sof(O97)=Sof(O98)=Sof(O99)=Sof(F100)=Sof(F101)=Sof(F102)=
 FVAR(1)
 Sof(S76)=Sof(C80)=Sof(O77)=Sof(O78)=Sof(O79)=Sof(F81)=Sof(F82)=Sof(F83)=1-
 FVAR(2)
 Sof(S1)=Sof(C69)=Sof(O70)=Sof(O71)=Sof(O72)=Sof(F73)=Sof(F74)=Sof(F75)=FVAR(2)
4.a Free rotating group:
 S1(C69,O70,O71,O72,F73,F74,F75), S76(C80,O77,O78,O79,F81,F82,F83), S103(C96,
 O97,O98,O99,F100,F101,F102), S8AA(C96A,O97A,O98A,O104,F1,F2,F105), S52(F57,F58,
 F59,O53,O54,O55,C56), S60(F65,F66,F67,O61,O62,O63,C64)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C29(H29),
 C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41),
  C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50)
4.c Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C108(H10D,H10E,H10F)
;
_shelx_res_checksum              31363
_shelx_hkl_checksum              79736
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'