Structural diversity in Ni(II) cluster chemistry: Ni5, Ni6, and {NiNa2}n complexes bearing the Schiff-base ligand N-naphthalidene-2-amino-5-chlorobenzoic acid.
Perlepe, Panagiota S.; Cunha-Silva, Luís; Bekiari, Vlasoula; Gagnon, Kevin J.; Teat, Simon J.; Escuer, Albert; Stamatatos, Theocharis C.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10256–10270; doi:10.1039/c6dt01162d

data_7040188
_publ_section_title
;
 Structural diversity in Ni(II) cluster chemistry: Ni5, Ni6, and {NiNa2}n
 complexes bearing the Schiff-base ligand
 N-naphthalidene-2-amino-5-chlorobenzoic acid.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10256
_journal_page_last               10270
_journal_paper_doi               10.1039/c6dt01162d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C116 H96 Cl10 N6 Ni6 O27.29'
_chemical_formula_weight         2717.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-01-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.5171(11)
_cell_length_b                   27.7084(10)
_cell_length_c                   31.0222(12)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.099
_cell_measurement_theta_min      2.2955
_cell_volume                     23653.0(16)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            226986
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.191
_diffrn_reflns_theta_max         24.191
_diffrn_reflns_theta_min         2.149
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS, Madison WI'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       lath
_exptl_crystal_F_000             11123
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.017
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1537
_refine_ls_number_reflns         14570
_refine_ls_number_restraints     584
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+329.1099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1958
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11211
_reflns_number_total             14570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01162d1.cif
_cod_data_source_block           comp_6
_cod_database_code               7040188
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              21181
_shelx_fab_checksum              54207