Crystal structure of tricarbonyl(<i>N</i>-diphenylphosphanyl-<i>N</i>,<i>N</i>'-diisopropyl-<i>P</i>-phenylphosphonous diamide-κ^2^<i>P</i>,<i>P</i>')cobalt(I) tetracarbonylcobaltate({-}I) toluene 0.25-solvate
Dura, Laura; Spannenberg, Anke; Beweries, Torsten; Acta Crystallographica Section E 70 (2014) 533–535; doi:10.1107/S1600536814024908

data_2240229
_publ_section_title
;
 Crystal structure of
 tricarbonyl(<i>N</i>-diphenylphosphanyl-<i>N</i>,<i>N</i>'-diisopropyl-<i>P</i>-phenylphosphonous
 diamide-\k^2^<i>P</i>,<i>P</i>')cobalt(I) tetracarbonylcobaltate({-}I)
 toluene 0.25-solvate
;
_journal_coeditor_code           RZ5139
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              533
_journal_page_last               535
_journal_paper_doi               10.1107/S1600536814024908
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Co (C24 H30 N2 P2) (C O)3] [Co (C O)4], 0.25C7 H8'
_chemical_formula_moiety         'C27 H30 Co N2 O3 P2, C4 Co O4, 0.25(C7 H8)'
_chemical_formula_sum            'C32.75 H32 Co2 N2 O7 P2'
_chemical_formula_weight         745.40
_chemical_name_systematic
;Tricarbonyl(<i>N</i>-diphenylphosphanyl-<i>N</i>,<i>N</i>'-diisopropyl-<i>P</i>-phenylphosphonous diamide-\k^2^<i>P</i>,<i>P</i>')cobalt(I)
tetracarbonylcobaltate(-I) toluene 0.25-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 103.9330(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1602(6)
_cell_length_b                   12.9730(3)
_cell_length_c                   24.7883(6)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      3.67
_cell_volume                     6916.6(3)
_computing_cell_refinement
;
SAINT (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            89837
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.498
_diffrn_reflns_theta_min         2.403
_exptl_absorpt_coefficient_mu    8.790
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.12
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2011)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       needle
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.572
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         12171
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0494P)^2^+7.7784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                11080
_reflns_number_total             12171
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5139sup1.cf
_cod_data_source_block           I
_cod_database_code               2240229
_cod_database_fobs_code          2240229
_shelx_hkl_checksum              8887
_shelx_res_checksum              84862