Evaluating Molecular Cobalt Complexes for the Conversion of N2 to NH3.
Del Castillo, Trevor J.; Thompson, Niklas B.; Suess, Daniel L. M.; Ung, Gaël; Peters, Jonas C.; Inorganic chemistry 54 (2015) 9256–9262; doi:10.1021/acs.inorgchem.5b00645

data_4343073
_publ_section_title
;
 Evaluating Molecular Cobalt Complexes for the Conversion of N2 to NH3.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9256
_journal_page_last               9262
_journal_paper_doi               10.1021/acs.inorgchem.5b00645
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C39 H60 Cl Co N P3, C24 H20 B'
_chemical_formula_sum            'C63 H80 B Cl Co N P3'
_chemical_formula_weight         1049.38
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.11 svn.r2872 for OlexSys, GUI svn.r4765)
;
_cell_angle_alpha                83.935(3)
_cell_angle_beta                 79.063(3)
_cell_angle_gamma                89.303(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9491(7)
_cell_length_b                   14.9096(10)
_cell_length_c                   17.8512(11)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.67
_cell_measurement_theta_min      2.33
_cell_volume                     2845.1(3)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0972
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            103727
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.630
_diffrn_reflns_theta_min         1.373
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0781 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.8254.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       plate
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         15990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0375P)^2^+0.8344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10280
_reflns_number_total             15990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00645_si_002.cif
_cod_data_source_block           F_NArPCoClBPh4
_cod_depositor_comments
'Adding full bibliography for 4343069--4343073.cif.'
_cod_database_code               4343073
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C37(H37), C25(H25), C34(H34), C31(H31), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C2(H2), C9(H9), C16(H16), C19(H19), C10(H10), C3(H3), C5(H5),
 C12(H12), C57(H57), C47(H47), C41(H41), C61(H61), C53(H53), C60(H60), C49(H49),
  C51(H51), C63(H63), C54(H54), C50(H50), C45(H45), C43(H43), C56(H56),
 C42(H42), C48(H48), C44(H44), C55(H55), C62(H62), C59(H59)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C27(H27A,
 H27B,H27C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C), C35(H35A,H35B,H35C),
 C33(H33A,H33B,H33C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              67656
_shelx_hkl_checksum              37797