Synthesis and Crystal Structure of a Hexa-DMF Nickel(II) Complex that Belongs to an S6 Point Group
YAMAGUCHI, Ryo; YAMASAKI, Mikio; SAKIYAMA, Hiroshi; X-ray Structure Analysis Online 27 (2011) 71–; doi:10.2116/xraystruct.27.71

data_1551724
_publ_section_title
;
 Synthesis and Crystal Structure of a Hexa-DMF Nickel(II) Complex that
 Belongs to an S6 Point Group
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              71
_journal_paper_doi               10.2116/xraystruct.27.71
_journal_volume                  27
_journal_year                    2011
_chemical_formula_moiety         'C18 H42 N6 Ni O6, 2(C24 H20 B)'
_chemical_formula_sum            'C66 H82 B2 N6 Ni O6'
_chemical_formula_weight         1135.73
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   30.2714(5)
_cell_length_b                   9.26438(10)
_cell_length_c                   22.0462(4)
_cell_measurement_reflns_used    61221
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      3.54
_cell_volume                     6182.76(17)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68928
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2424.00
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.200
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  5415 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.057(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11242
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.8770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                10339
_reflns_number_total             11242
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            27_71_1.cif
_cod_data_source_block           sc0907
_cod_original_cell_volume        6182.75(17)
_cod_database_code               1551724