Reactivity of Hydride Bridges in High-Spin [3M-3(μ-H)] Clusters (M = Fe(II), Co(II)).
Lee, Yousoon; Anderton, Kevin J.; Sloane, Forrest T.; Ermert, David M.; Abboud, Khalil A.; García-Serres, Ricardo; Murray, Leslie J.; Journal of the American Chemical Society  (2015) 150817071736007–; doi:10.1021/jacs.5b05204

data_4124383
_publ_section_title
;
 Reactivity of Hydride Bridges in High-Spin [3M-3(\m-H)] Clusters (M =
 Fe(II), Co(II)).
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150817071736007
_journal_paper_doi               10.1021/jacs.5b05204
_journal_year                    2015
_chemical_formula_moiety         'C45 H66 N6 Co3, C7 H8'
_chemical_formula_sum            'C52 H74 Co3 N6'
_chemical_formula_weight         959.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-01-14 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 112.3383(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6868(16)
_cell_length_b                   11.4465(9)
_cell_length_c                   22.040(2)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     4827.2(7)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL-2014 (Bruker, 2014)'
_computing_publication_material  'SHELXTL-2014 (Bruker, 2014)'
_computing_structure_refinement  'SHELXTL-2014 (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2014 (Bruker, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48194
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.073
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.9518
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       plates
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Flack x determined using 4854 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         11089
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.997
_reflns_friedel_fraction_full    0.997
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                10265
_reflns_number_total             11089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05204_si_003.cif
_cod_data_source_block           kand5
_cod_original_cell_volume        4827.1(8)
_cod_database_code               4124383
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2014/6
_shelx_res_checksum              4896
_shelx_hkl_checksum              19184