The tetrahedral tetrakis(phosphine) complex [bis(diphenylphosphino)butane-κ<i>P,P</i>]nickel(0)‒benzene (1/2.5)
Alison J. Edwards; Mikael Retbøll; Eric Wenger; Acta Crystallographica Section E 58 (2002) m375–m377; doi:10.1107/S1600536802011121

data_2201541
_publ_section_title
;
 The tetrahedral tetrakis(phosphine) complex
 [bis(diphenylphosphino)butane-\k<i>P,P</i>]nickel(0)--benzene (1/2.5)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m375
_journal_page_last               m377
_journal_paper_doi               10.1107/S1600536802011121
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ni (C28 H2 8P2)2], 2.5C6 H6'
_chemical_formula_moiety         'C56 H56 Ni P4, 2.5C6 H6'
_chemical_formula_sum            'C71 H71 Ni P4'
_chemical_formula_weight         1106.955
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.5142(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9938(5)
_cell_length_b                   11.7063(4)
_cell_length_c                   27.1914(9)
_cell_measurement_reflns_used    37457
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.91
_cell_volume                     5920.8(3)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
CAMERON (Watkin et al., 1996)
;
_computing_publication_material
;
CRYSTALS and maXus (Mackay et al., 1999)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al., 2001)
;
_computing_structure_solution
;
SIR97 (Altomare et al., 1999)
;
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65297
_diffrn_reflns_theta_full        25.4
_diffrn_reflns_theta_max         25.4
_diffrn_reflns_theta_min         3.0
_exptl_absorpt_coefficient_mu    0.48
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens, 1970)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2339
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         2785
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Weighting scheme: Chebychev polynomial with three parameters
(Carruthers & Watkin, 1979); 11.3, -0.949 and 5.26
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                2785
_reflns_number_total             10780
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6135.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2201541
_cod_database_fobs_code          2201541