Complexes of MN2S2·Fe(η(5)-C5R5)(CO) as platform for exploring cooperative heterobimetallic effects in HER electrocatalysis.
Ghosh, Pokhraj; Quiroz, Manuel; Wang, Ning; Bhuvanesh, Nattamai; Darensbourg, Marcetta Y.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5617–5624; doi:10.1039/c6dt04666e

data_7041977
_publ_section_title
;
 Complexes of MN2S2&#x00B7;Fe(\h(5)-C5R5)(CO) as platform for exploring
 cooperative heterobimetallic effects in HER electrocatalysis.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5617
_journal_page_last               5624
_journal_paper_doi               10.1039/c6dt04666e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C20 H33 Co Fe N3 O2 S2, 2(F3 P0.5)'
_chemical_formula_sum            'C20 H33 Co F6 Fe N3 O2 P S2'
_chemical_formula_weight         671.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-06 deposited with the CCDC.
2017-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.649(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.3067(9)
_cell_length_b                   21.8234(9)
_cell_length_c                   10.8799(6)
_cell_measurement_reflns_used    9612
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      26.462
_cell_measurement_theta_min      2.473
_cell_volume                     5187.3(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            227516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.162
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.7352
_exptl_absorpt_correction_T_min  0.6634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0975 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.9023.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0051P)^2^+42.8888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4020
_reflns_number_total             4560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04666e2.cif
_cod_data_source_block           comcp
_cod_depositor_comments
'Adding full bibliography for 7041975--7041978.cif.'
_cod_database_code               7041977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C13 \\sim C12 \\sim C11 \\sim C17: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C13, C12, C11, C17
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
4.b 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)
;
_shelx_res_checksum              79989
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'