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_7040184
_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_moiety         'C84 H70 Cl4 N8 Ni5 O18, 3(C3 H7 N O)'
_chemical_formula_sum            'C93 H91 Cl4 N11 Ni5 O21'
_chemical_formula_weight         2134.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             '19 May 2016'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                92.408(2)
_cell_angle_beta                 99.389(2)
_cell_angle_gamma                116.998(2)
_cell_formula_units_Z            1
_cell_length_a                   14.1417(10)
_cell_length_b                   14.1587(10)
_cell_length_c                   14.7117(11)
_cell_measurement_reflns_used    8253
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.62
_cell_volume                     2566.8(3)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20519
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.977
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       plate
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.699
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         8395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0974
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+26.5167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7062
_reflns_number_total             8395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01162d1.cif
_cod_data_source_block           comp2_rev
_cod_database_code               7040184
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              85167