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_7040185
_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
'C78 H58 Cl5 N5 Ni5 O16, C4 H10 O, 3(C2 H3 N), 4(C H4 O)'
_chemical_formula_sum            'C94 H96 Cl5 N9 Ni5 O21'
_chemical_formula_weight         2158.59
_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   mixed
_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                69.585(9)
_cell_angle_beta                 84.074(9)
_cell_angle_gamma                65.021(9)
_cell_formula_units_Z            2
_cell_length_a                   17.414(4)
_cell_length_b                   17.728(4)
_cell_length_c                   18.040(4)
_cell_measurement_reflns_used    9304
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.64
_cell_measurement_theta_min      2.55
_cell_volume                     4724.8(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            128931
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       plate
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.387
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.728
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1164
_refine_ls_number_reflns         21557
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.728
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0963P)^2^+16.5262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18848
_reflns_number_total             21557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01162d1.cif
_cod_data_source_block           comp3_rev
_cod_original_cell_volume        4724.9(19)
_cod_database_code               7040185
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.708
_shelx_estimated_absorpt_t_max   0.870
_shelx_res_checksum              2936
_shelx_fab_checksum              27243