Chlorido(1-pyrrolidinecarbodithioato-κ^2^<i>S</i>,<i>S</i>')(triphenylphosphine-κ<i>P</i>)nickel(II) chloroform hemisolvate
Kropidłowska, Anna; Janczak, Jan; Gołaszewska, Jolanta; Becker, Barbara; Acta Crystallographica Section E 63 (2007) m1947–m1947; doi:10.1107/S1600536807027791

data_2214274
_publ_section_title
;Chlorido(1-pyrrolidinecarbodithioato-\k^2^<i>S</i>,<i>S</i>')(triphenylphosphine-\k<i>P</i>)nickel(II)
 chloroform hemisolvate
;
_journal_coeditor_code           IM2018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1947
_journal_page_last               m1947
_journal_paper_doi               10.1107/S1600536807027791
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Ni (C5 H8 N S2) Cl (C18 H15 P)], 0.5C H Cl3'
_chemical_formula_moiety         'C23 H23 Cl N Ni P S2, 0.5(C H Cl3)'
_chemical_formula_sum            'C47 H47 Cl5 N2 Ni2 P2 S4'
_chemical_formula_weight         1124.72
_chemical_name_systematic
;
Chlorido(1-pyrrolidinecarbodithioato-\k^2^S,S')(triphenylphosphine-
\kP)nickel(II) chloroform hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.37(2)
_cell_angle_beta                 91.21(2)
_cell_angle_gamma                117.39(2)
_cell_formula_units_Z            1
_cell_length_a                   9.713(2)
_cell_length_b                   10.076(2)
_cell_length_c                   14.509(3)
_cell_measurement_reflns_used    876
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.72
_cell_volume                     1260.3(5)
_computing_cell_refinement       'CrysAlis CCD'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Kuma KM-4 with CCD area detector'
_diffrn_measurement_method       \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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16395
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(face-indexed) (SHELXTL; Sheldrick, 1990)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      1.48
_exptl_crystal_density_method    floatation
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.507
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0012
_refine_ls_R_factor_all          0.1597
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                3417
_reflns_number_total             6060
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2018.cif
_cod_data_source_block           I
_cod_database_code               2214274
_cod_database_fobs_code          2214274