Synthesis and Crystal Structure of the Nickel(II) Phosphoranide Complex trans-(PMe~3~)~2~[(C~4~H~6~O~3~)~2~P-P]NiCl
Richard Faw; Craig D. Montgomery; Steven J. Rettig; Bryn Shurmer; Inorganic Chemistry 37 (1998) 4136–4138; doi:10.1021/ic980193f

data_4322931
_publ_contact_author_email       ' montgome@twu.ca '
_publ_contact_author_fax         ' 604-513-2018 '
_publ_contact_author_name        ' Craig Montgomery'
_publ_contact_author_phone       ' 604-888-7511 ext 3210 '
_publ_section_title
;
 Synthesis and Crystal Structure of the Nickel(II) Phosphoranide Complex
 trans-(PMe~3~)~2~[(C~4~H~6~O~3~)~2~P-P]NiCl
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4136
_journal_page_last               4138
_journal_paper_doi               10.1021/ic980193f
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C14 H30 Cl O6 Ni P3 '
_chemical_formula_sum            'C14 H30 Cl Ni O6 P3'
_chemical_formula_weight         481.46
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_date             1998-01-09
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8221(7)
_cell_length_b                   9.3525(10)
_cell_length_c                   13.3040(4)
_cell_measurement_reflns_used    16113
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     2217.5(3)
_computing_cell_refinement       'd*TREK (MSC, 1997)'
_computing_data_collection       'd*TREK (MSC, 1997)'
_computing_data_reduction        'd*TREK (MSC, 1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      180.2
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03331
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20339
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.14
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  1.003
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.51
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.365
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0717
_reflns_number_gt                '5039 (includes Friedel pairs)'
_reflns_number_total             3376
_reflns_threshold_expression     I>0.00\s(I)
_cod_data_source_file            ic980193f.cif
_cod_data_source_block           IC980193F
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C14 H30 Cl O6 Ni P3 '
_cod_database_code               4322931