[1,2-Bis(diphenylphosphino)ethane-κ^2^<i>P</i>,<i>P</i>'](2-carboxylatothiophenolato-κ^2^<i>O</i>,<i>S</i>)nickel(II) methanol solvate
Miao, Jinling; Li, Furong; Chen, Haiyan; Wang, Daqi; Nie, Yong; Acta Crystallographica Section E 65 (2009) m156–; doi:10.1107/S1600536808044280

data_2220913
_publ_section_title
;[1,2-Bis(diphenylphosphino)ethane-\k^2^<i>P</i>,<i>P</i>'](2-carboxylatothiophenolato-\k^2^<i>O</i>,<i>S</i>)nickel(II)
 methanol solvate
;
_journal_coeditor_code           SJ2555
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m156
_journal_paper_doi               10.1107/S1600536808044280
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C7 H4 O2 S) (C26 H24 P2)] , C H4 O'
_chemical_formula_moiety         'C33 H28 Ni O2 P2 S , C H4 O'
_chemical_formula_sum            'C34 H32 Ni O3 P2 S'
_chemical_formula_weight         641.31
_chemical_name_systematic
;
[1,2-Bis(diphenylphosphino)ethane-\k^2^<i>P</i>,<i>P</i>'](2-
carboxylatothiophenolato-\k^2^<i>O</i>,<i>S</i>)nickel(II) methanol solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.085(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9229(15)
_cell_length_b                   11.6244(10)
_cell_length_c                   19.553(2)
_cell_measurement_reflns_used    3936
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.984
_cell_measurement_theta_min      2.297
_cell_volume                     3115.7(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14599
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7781
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0402P)^2^+2.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                3538
_reflns_number_total             5484
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2555.cif
_cod_data_source_block           I
_cod_original_cell_volume        3115.6(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220913
_cod_database_fobs_code          2220913