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_7041975
_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         'C16 H23 Co Fe N3 O3 S2, C H2 Cl2, B F4'
_chemical_formula_sum            'C17 H25 B Cl2 Co F4 Fe N3 O3 S2'
_chemical_formula_weight         656.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2016-12-06 deposited with the CCDC.
2017-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                73.506(3)
_cell_angle_beta                 75.942(3)
_cell_angle_gamma                83.232(3)
_cell_formula_units_Z            2
_cell_length_a                   7.592(2)
_cell_length_b                   12.668(3)
_cell_length_c                   13.662(4)
_cell_measurement_reflns_used    4883
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.530
_cell_measurement_theta_min      2.603
_cell_volume                     1220.5(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.967
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10561
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         1.594
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0727 before and 0.0358 after correction.
The Ratio of minimum to maximum transmission is 0.7142.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5441
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0420P)^2^+0.5891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             5441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04666e2.cif
_cod_data_source_block           cofe2co
_cod_depositor_comments
'Adding full bibliography for 7041975--7041978.cif.'
_cod_database_code               7041975
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.626
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Co1-N3A \\sim Co1-N3
 with sigma of 0.02
 O1-N3 \\sim O1A-N3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Co1 \\sim N3 \\sim N3A \\sim O1A \\sim O1: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Co1, N3, N3A, O1A, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1A)=Sof(N3A)=1-FVAR(1)
 Sof(O1)=Sof(N3)=FVAR(1)
6.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), C1S(H1SA,H1SB)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              53528
_olex2_submission_special_instructions 'No special instructions were received'