An unprecedented example of a cis-phosphonodithioato nickel(ii) complex built by an extensive hydrogen bonding supramolecular network
Albano, Vincenzo G.; Aragoni, M. Carla; Arca, Massimiliano; Castellari, Carlo; Demartin, Francesco; Devillanova, Francesco A.; Isaia, Francesco; Lippolis, Vito; Loddo, Laura; Verani, Gaetano; Chemical Communications  (2002) 1170–; doi:10.1039/b200414c

data_7114381
_publ_section_title
;
 An unprecedented example of a cis-phosphonodithioato nickel(ii) complex
 built by an extensive hydrogen bonding supramolecular network
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              1170
_journal_paper_doi               10.1039/b200414c
_journal_year                    2002
_chemical_formula_sum            'C9 H15 N2 O P S2'
_chemical_formula_weight         262.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4077(13)
_cell_length_b                   6.1908(5)
_cell_length_c                   13.7291(12)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      3.2
_cell_volume                     1224.56(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD Smart diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.1323
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16240
_diffrn_reflns_theta_full        32.22
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   'theta dependent correction'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                2742
_reflns_number_total             4052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200414c.txt
_cod_data_source_block           compound_2
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-08-09
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_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7114381