Cooperative activation of O-H and S-H bonds across the Co-P bond of an N-heterocyclic phosphido complex.
Poitras, Andrew M.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3074–3079; doi:10.1039/c8dt05052j

data_7048927
_publ_section_title
;
 Cooperative activation of O-H and S-H bonds across the Co-P bond of an
 N-heterocyclic phosphido complex.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3074
_journal_page_last               3079
_journal_paper_doi               10.1039/c8dt05052j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C47 H47.00 Co1 N2 O1 P4'
_chemical_formula_sum            'C47 H47 Co N2 O P4'
_chemical_formula_weight         838.73
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-20
_audit_creation_method           CRYSTALS_ver_14.61_build_00000
_audit_update_record
;
2018-11-02 deposited with the CCDC.
2019-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                80.067(3)
_cell_angle_beta                 75.461(3)
_cell_angle_gamma                77.245(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4224(7)
_cell_length_b                   12.7223(7)
_cell_length_c                   16.9771(10)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2311.2(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.052
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13466
_diffrn_reflns_theta_full        30.042
_diffrn_reflns_theta_max         30.042
_diffrn_reflns_theta_min         1.654
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             876
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and n-pentane'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_platon_squeeze_details
;
TITL ap_1_52_0m in P-1
CELL   11.4220   12.7220   16.9770     80.07     75.46     77.25
SPGR P-1
C101 0.063 0.103 0.315 !       5.51 eA-3
C102 0.126 0.289 0.239 !       5.00 eA-3
C103 0.188 0.079 0.283 !       4.83 eA-3
C104 0.266 0.131 0.250 !       4.80 eA-3
C105 0.014 0.211 0.293 !       4.36 eA-3
C106 0.231 0.253 0.218 !       4.07 eA-3
C107 0.281 0.340 0.181 !       3.69 eA-3
C108 0.348 0.265 0.201 !       3.29 eA-3
C109 0.358 0.149 0.235 !       3.13 eA-3
C110 0.139 0.182 0.263 !       2.63 eA-3
Q111 0.253 0.557 0.166 !       1.27 eA-3
Q112 0.308 0.533 0.229 !       0.96 eA-3
Q113 0.138 0.561 0.171 !       0.95 eA-3
C114 1.005 0.069 0.351 !       0.89 eA-3
Q115 0.327 0.858 0.044 !       0.86 eA-3
Q116 0.343 0.861 0.129 !       0.85 eA-3
Q117 0.763 0.425 0.279 !       0.75 eA-3
Q118 0.629 0.096 0.186 !       0.69 eA-3
Q119 0.436 0.818 0.136 !       0.66 eA-3
Q120 0.624 0.743 0.313 !       0.62 eA-3
Q121 0.664 0.410 0.284 !       0.60 eA-3
Q122 0.937 0.838 0.076 !       0.59 eA-3
Q123 0.656 0.463 0.019 !       0.56 eA-3
Q124 0.657 0.144 0.279 !       0.52 eA-3
Q125 0.666 0.135 0.219 !       0.51 eA-3
;
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         13466
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0120280
_refine_ls_shift/su_mean         0.0002453
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 1.87P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1144
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1144
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                10016
_reflns_number_total             13466
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0600
_oxford_refine_ls_scale          0.14248(4)
_oxford_reflns_number_all        13466
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ap_1_52_0m in P-1'
_cod_data_source_file            c8dt05052j2.cif
_cod_data_source_block           ap_1_52
_cod_depositor_comments          'Adding full bibliography for 7048927.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C47 H47.00 Co1 N2 O1 P4'
_cod_database_code               7048927
_platon_squeeze_void_probe_radius 1.20