Reinvestigation of Water Oxidation Catalyzed by a Dinuclear Cobalt Polypyridine Complex: Identification of CoOxas a Real Heterogeneous Catalyst
Wang, Jia-Wei; Sahoo, Pathik; Lu, Tong-Bu; ACS Catalysis  (2016) 5062–; doi:10.1021/acscatal.6b00798

data_4513902
_publ_section_title
;
 Reinvestigation of Water Oxidation Catalyzed by a Dinuclear Cobalt
 Polypyridine Complex: Identification of CoOxas a Real Heterogeneous
 Catalyst
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              5062
_journal_paper_doi               10.1021/acscatal.6b00798
_journal_year                    2016
_chemical_formula_moiety         'C32 H45 Co2 N8 O2.7, 3(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C32 H48.9 Cl3 Co2 N8 O16.71'
_chemical_formula_weight         1037.26
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.871(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2143(3)
_cell_length_b                   12.64794(18)
_cell_length_c                   19.3370(4)
_cell_measurement_reflns_used    34737
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.6370
_cell_measurement_theta_min      2.7550
_cell_volume                     4134.10(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5058
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
  1 omega  -86.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6093  -38.0000   60.0000 99

  2 omega  -36.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6093   38.0000  -30.0000 99

  3 omega -100.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6093 -178.0000 -180.0000 65

  4 omega  -85.00   17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6093  -57.0000   30.0000 102

  5 omega  -16.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6875   57.0000  -30.0000 100

  6 omega  -51.00   -4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6875  136.0000   56.0000 47

  7 omega  -60.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6875  -57.0000 -180.0000 100

  8 omega  -40.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6093   57.0000   30.0000 102

  9 omega  -86.00  -61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6093  -38.0000  150.0000 25

 10 omega   24.00   73.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6875 -134.0000  171.0000 49

 11 omega   53.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6875 -178.0000  150.0000 46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0084389000
_diffrn_orient_matrix_UB_12      0.0217111000
_diffrn_orient_matrix_UB_13      -0.0359793000
_diffrn_orient_matrix_UB_21      -0.0183139000
_diffrn_orient_matrix_UB_22      -0.0480726000
_diffrn_orient_matrix_UB_23      -0.0164271000
_diffrn_orient_matrix_UB_31      -0.0367962000
_diffrn_orient_matrix_UB_32      0.0189331000
_diffrn_orient_matrix_UB_33      -0.0003713000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            90759
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.942
_diffrn_reflns_theta_min         2.766
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       plate
_exptl_crystal_F_000             2142
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0778P)^2^+9.9667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8615
_reflns_number_total             11046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b00798_si_002.cif
_cod_data_source_block           exp_8737
_cod_original_cell_volume        4134.11(14)
_cod_original_formula_sum        'C32 H48.90 Cl3 Co2 N8 O16.71'
_cod_database_code               4513902
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H32(0.044) H17(0.048) H23A(0.066) H23B(0.066) H23C(0.066)
 H18(0.064) H1(0.055) H13(0.069) H31(0.058) H30(0.069) H19(0.083) H4(0.078)
 H8A(0.065) H8B(0.065) H20(0.082) H14(0.082) H29(0.068) H16(0.057) H22A(0.059)
 H22B(0.059) H15(0.078) H10A(0.077) H10B(0.077) H10C(0.077) H11A(0.057)
 H11B(0.057) H2(0.075) H9A(0.062) H9B(0.062) H26A(0.082) H26B(0.082)
 H26C(0.082) H27A(0.06) H27B(0.06) H6A(0.065) H6B(0.065) H3(0.082) H7A(0.095)
 H7B(0.095) H7C(0.095) H24A(0.063) H24B(0.063) H25A(0.062) H25B(0.062)
 H1WA(0.13) H1WB(0.13) H2WA(0.176) H2WB(0.176) H1A(0.053)
 Fixed X: H32(0.4178) H17(0.091) H23A(0.3321) H23B(0.3773) H23C(0.3593) H18(-
 0.0375) H1(0.3255) H13(-0.0322) H31(0.5456) H30(0.5656) H19(-0.0599)
 H4(0.5223) H8A(0.3306) H8B(0.2971) H20(0.047) H14(-0.0675) H29(0.4594)
 H16(0.1593) H22A(0.1871) H22B(0.2219) H15(0.0322) H10A(0.2029) H10B(0.2879)
 H10C(0.2261) H11A(0.1046) H11B(0.0839) H2(0.4557) H9A(0.168) H9B(0.2045)
 H26A(0.175) H26B(0.1309) H26C(0.1514) H27A(0.3202) H27B(0.2825) H6A(0.4118)
 H6B(0.3843) H3(0.5554) H7A(0.2108) H7B(0.2634) H7C(0.2991) H24A(0.2602)
 H24B(0.1817) H25A(0.258) H25B(0.3336) H1WA(0.3584) H1WB(0.2871) H2WA(0.1839)
 H2WB(0.2079)
 Fixed Y: H32(0.6948) H17(0.7086) H23A(0.4477) H23B(0.4692) H23C(0.5651)
 H18(0.6995) H1(0.8714) H13(0.9934) H31(0.6997) H30(0.651) H19(0.6149)
 H4(0.9673) H8A(1.109) H8B(1.1473) H20(0.5444) H14(0.8884) H29(0.5869)
 H16(0.7952) H22A(0.4708) H22B(0.5878) H15(0.8003) H10A(1.1329) H10B(1.0862)
 H10C(1.0149) H11A(0.9673) H11B(1.076) H2(0.885) H9A(1.1022) H9B(1.1824)
 H26A(0.4606) H26B(0.4873) H26C(0.5801) H27A(0.4992) H27B(0.6157) H6A(1.0067)
 H6B(0.8853) H3(0.9337) H7A(1.0108) H7B(0.9079) H7C(1.0231) H24A(0.3563)
 H24B(0.4144) H25A(0.3665) H25B(0.4268) H1WA(0.7866) H1WB(0.7681) H2WA(0.8425)
 H2WB(0.7678)
 Fixed Z: H32(0.2676) H17(0.2597) H23A(0.1517) H23B(0.2389) H23C(0.181)
 H18(0.1703) H1(0.4026) H13(0.1231) H31(0.3586) H30(0.4802) H19(0.057)
 H4(0.3184) H8A(0.2514) H8B(0.166) H20(0.0337) H14(0.0154) H29(0.5079)
 H16(0.0801) H22A(0.0962) H22B(0.098) H15(-0.0096) H10A(0.3372) H10B(0.347)
 H10C(0.3673) H11A(0.2762) H11B(0.2301) H2(0.4874) H9A(0.1541) H9B(0.2229)
 H26A(0.3847) H26B(0.2981) H26C(0.3586) H27A(0.4463) H27B(0.4342) H6A(0.1952)
 H6B(0.1816) H3(0.4435) H7A(0.0736) H7B(0.0777) H7C(0.0758) H24A(0.2155)
 H24B(0.2149) H25A(0.3381) H25B(0.3334) H1WA(0.5955) H1WB(0.5368) H2WA(0.4514)
 H2WB(0.4113)
;
_shelx_res_checksum              10490
_shelx_hkl_checksum              68569
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'