An Unsymmetrical Trinickel Metal Complex with 4-Sulfobenzoate Axial Ligand: [Ni3(dpa)4(4-sb)(H2O)]x3H2O
Zheng, Xiao-Feng; Zhu, Long-Guan; Crystals 1 (2011) 120–127; doi:10.3390/cryst1030120

data_1508363
_publ_section_title
;
 An Unsymmetrical Trinickel Metal Complex with 4-Sulfobenzoate Axial
 Ligand: [Ni3(dpa)4(4-sb)(H2O)]x3H2O
;
_journal_issue                   3
_journal_name_full               Crystals
_journal_page_first              120
_journal_page_last               127
_journal_paper_doi               10.3390/cryst1030120
_journal_volume                  1
_journal_year                    2011
_chemical_formula_moiety         '2(C47 H38 N12 Ni3 O6 S), 7(O)'
_chemical_formula_sum            'C94 H88 N24 Ni6 O19 S2'
_chemical_formula_weight         2274.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5250(14)
_cell_length_b                   22.703(2)
_cell_length_c                   31.993(3)
_cell_measurement_reflns_used    13436
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      3.14
_cell_volume                     11276.4(18)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART area-detector diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.1197
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            67491
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.8896
_exptl_absorpt_correction_T_min  0.8116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9942
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+30.1858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2600
_reflns_number_gt                5213
_reflns_number_total             9942
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            crystals-01-00120-s001.cif
_cod_data_source_block           o
_cod_database_code               1508363