Cooperative H2 Activation across a Metal‒Metal Multiple Bond and Hydrogenation Reactions Catalyzed by a Zr/Co Heterobimetallic Complex
Gramigna, Kathryn M.; Dickie, Diane A.; Foxman, Bruce M.; Thomas, Christine M.; ACS Catalysis 9 (2019) 3153–; doi:10.1021/acscatal.8b04390

data_4514740
_publ_section_title
;
 Cooperative H2 Activation across a Metal--Metal Multiple Bond and
 Hydrogenation Reactions Catalyzed by a Zr/Co Heterobimetallic Complex
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              3153
_journal_paper_doi               10.1021/acscatal.8b04390
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C32 H58 Co1 I1 N4 P2 Zr1'
_chemical_formula_sum            'C32 H58 Co I N4 P2 Zr'
_chemical_formula_weight         837.84
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-21
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4307(5)
_cell_length_b                   22.1735(8)
_cell_length_c                   10.8845(3)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3724.2(2)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27833
_diffrn_reflns_theta_full        29.994
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         1.837
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.37
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0380
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         5554
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.0018067
_refine_ls_shift/su_mean         0.0000555
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 4.40P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0668
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0668
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4954
_reflns_number_total             5554
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.64
_oxford_diffrn_Wilson_scale      288.06
_oxford_refine_ls_r_factor_ref   0.0333
_oxford_refine_ls_scale          0.063209(7)
_oxford_reflns_number_all        5554
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'kg_408_0ma in Pnma'
_cod_data_source_file            cs8b04390_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C32 H58 Co1 I1 N4 P2 Zr1'
_cod_database_code               4514740