Crystallization condition-controlled assembly of oxygen-bridged tetranuclear and hexanuclear Ni(ii) clusters: syntheses, structures and properties
Liu, Shizheng; Wang, Suna; Cao, Fan; Fu, Haiying; Li, Dacheng; Dou, Jianmin; RSC Adv. 2 (2012) 1310–; doi:10.1039/C2RA01219G

data_7238593
_publ_section_title
;
 Crystallization condition-controlled assembly of oxygen-bridged
 tetranuclear and hexanuclear Ni(ii) clusters: syntheses, structures and
 properties
;
_journal_issue                   4
_journal_name_full               'RSC Adv.'
_journal_page_first              1310
_journal_paper_doi               10.1039/C2RA01219G
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C73 H93 N11 Ni6 O17'
_chemical_formula_weight         1748.84
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_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                   27.556(3)
_cell_length_b                   16.8879(16)
_cell_length_c                   17.3304(19)
_cell_measurement_reflns_used    4338
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.1435
_cell_measurement_theta_min      2.2385
_cell_volume                     8064.9(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1438
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32407
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.8020
_exptl_absorpt_correction_T_min  0.5825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7131
_refine_ls_number_restraints     1276
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2091
_refine_ls_wR_factor_ref         0.2639
_reflns_number_gt                3284
_reflns_number_total             7131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra01219g.txt
_cod_data_source_block           100310b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        8065.0(14)
_cod_original_sg_symbol_H-M      'Pbcn '
_cod_database_code               7238593