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_7114359
_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
'Cu5 (C9 H10 N2 O2)4  (H S O4 )2  (C H4 O)2, 2(C H4 O)'
_chemical_formula_sum            'C40 H58 Cu5 N8 O20 S2'
_chemical_formula_weight         1352.76
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.989(7)
_cell_angle_beta                 64.844(6)
_cell_angle_gamma                68.106(6)
_cell_formula_units_Z            1
_cell_length_a                   11.002(4)
_cell_length_b                   11.393(4)
_cell_length_c                   11.863(4)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1248.5(8)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14707
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.264
_exptl_absorpt_correction_T_max  0.9356
_exptl_absorpt_correction_T_min  0.4312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs program'
_exptl_crystal_colour            black-green
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             691
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.534
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                5646
_reflns_number_total             7140
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b110799b.txt
_cod_data_source_block           exp2-38d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        1248.6(7)
_cod_database_code               7114359