Synthesis and structure of a heptanuclear nickel(ii) complex uniquely exhibiting four distinct binding modes, two of which are novel, for a hydroxamate ligand
Gaynor, Declan; Starikova, Zoya A.; Ostrovsky, Sergei; Haase, Wolfgang; Nolan, Kevin B.; Chemical Communications  (2002) 506–507; doi:10.1039/b110799b

data_7114360
_publ_section_title
;
 Synthesis and structure of a heptanuclear nickel(ii) complex uniquely
 exhibiting four distinct binding modes, two of which are novel, for a
 hydroxamate ligand
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              506
_journal_page_last               507
_journal_paper_doi               10.1039/b110799b
_journal_year                    2002
_chemical_formula_moiety         'C90 H120 N20 Ni7 O26 2+, S O4 2-, 15(H2 O)'
_chemical_formula_sum            'C90 H150 N20 Ni7 O45 S'
_chemical_formula_weight         2675.33
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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                   16.398(9)
_cell_length_b                   23.996(14)
_cell_length_c                   30.666(12)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.5
_cell_volume                     12067(11)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1998b)'
_computing_data_collection       'Bruker SMART (Bruker, 1998b)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1998b)'
_computing_molecular_graphics    'SHELXL PLUS ver. 5.10 (Bruker,1998a)'
_computing_publication_material  'SHELXL PLUS ver. 5.10 (Bruker, 1998a)'
_computing_structure_refinement  'SHELXL PLUS ver. 5.10 (Bruker, 1998a)'
_computing_structure_solution    'SHELXL PLUS ver. 5.10 (Bruker, 1998a)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SMART 1000 CCD'
_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  0.1354
_diffrn_reflns_av_sigmaI/netI    0.4306
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41850
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.9435
_exptl_absorpt_correction_T_min  0.7987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1998b)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983)'
_refine_ls_abs_structure_Flack   0.059(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.644
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         20598
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.649
_refine_ls_R_factor_all          0.1878
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0033P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                6247
_reflns_number_total             20598
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b110799b.txt
_cod_data_source_block           exp2.56(b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        12067(10)
_cod_database_code               7114360