Hydrogen Evolution Catalysis by a Sparsely Substituted Cobalt Chlorin
Maher, Andrew G.; Passard, Guillaume; Dogutan, Dilek K.; Halbach, Robert L.; Anderson, Bryce L.; Gagliardi, Christopher J.; Taniguchi, Masahiko; Lindsey, Jonathan S.; Nocera, Daniel G.; ACS Catalysis  (2017) 3597–; doi:10.1021/acscatal.7b00969

data_4514089
_publ_section_title
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 Hydrogen Evolution Catalysis by a Sparsely Substituted Cobalt Chlorin
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3597
_journal_paper_doi               10.1021/acscatal.7b00969
_journal_year                    2017
_chemical_formula_moiety         'C38 H34 Co N4'
_chemical_formula_sum            'C38 H34 Co N4'
_chemical_formula_weight         605.62
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2060(9)
_cell_length_b                   15.8073(7)
_cell_length_c                   19.2815(9)
_cell_measurement_reflns_used    90965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.97
_cell_volume                     5853.8(5)
_computing_cell_refinement       'SAINT 7.64A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS,2009)'
_computing_data_reduction        'SAINT 7.64A (Bruker-AXS, 2009)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            96101
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.8796
_exptl_absorpt_correction_T_min  0.8199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+3.6805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                4740
_reflns_number_total             6477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs7b00969_si_002.cif
_cod_data_source_block           1-Co
_cod_database_code               4514089
_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.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C20(H20), C15(H15), C13(H13), C12(H12), C34(H34), C31(H31),
 C8(H8), C7(H7), C22(H22), C23(H23), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C33(H33A,H33B,
 H33C), C30(H30A,H30B,H30C), C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'