A five-coordinate cobalt bis(dithiolene)‒phosphine complex [Co(pdt)~2~(PTA)] (pdt = phenyldithiolene; PTA = 1,3,5-triaza-7-phosphaadamantane)
Williams, DaShawn; Brannon, Jacob P.; Chandrasekaran, Perumalreddy; Stieber, S. Chantal E.; Acta Crystallographica Section E 76 (2020) 736–741; doi:10.1107/S2056989020005447

data_2243376
_publ_section_title
;
 A five-coordinate cobalt bis(dithiolene)--phosphine complex
 [Co(pdt)~2~(PTA)] (pdt = phenyldithiolene; PTA =
 1,3,5-triaza-7-phosphaadamantane)
;
_journal_coeditor_code           ZL2776
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              736
_journal_page_last               741
_journal_paper_doi               10.1107/S2056989020005447
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Co (C14 H10 S2)2 (C6 H12 N3 P), 0.5C2 H4 Cl2'
_chemical_formula_moiety         'C34 H32 Co N3 P S4, 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C35 H34 Cl Co N3 P S4'
_chemical_formula_weight         750.24
_chemical_name_systematic
;Bis(1,2-diphenyl-2-sulfanylideneethanethiolato-\k^2^<i>S</i>,<i>S</i>')(1,3,5-triaza-7-phosphaadamantane-\k<i>P</i>)cobalt(II)
dichloromethane hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                97.074(3)
_cell_angle_beta                 94.680(3)
_cell_angle_gamma                107.354(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0954(7)
_cell_length_b                   13.4319(9)
_cell_length_c                   14.7905(10)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      34.93
_cell_measurement_theta_min      3.54
_cell_volume                     1698.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and SHELXL2017 (Sheldrick,
2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      113.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Kappa'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.133
_diffrn_reflns_theta_min         2.593
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.571
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.8472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                6778
_reflns_number_total             7487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2776sup1.cif
_cod_data_source_block           I
_cod_database_code               2243376
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.885
_shelx_hkl_checksum              17649
_shelx_res_checksum              35852
_cod_database_fobs_code 2243376