Cyano-bridged Homodinuclear Copper(II) Complexes
Mihail Atanasov; Peter Comba; Graeme R. Hanson; Sascha Hausberg; Stefan Helmle; Hubert Wadepohl; Inorganic Chemistry 50 (2011) 6890–6901; doi:10.1021/ic102430a

data_4325724
_publ_section_title
;
 Cyano-bridged Homodinuclear Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6890
_journal_page_last               6901
_journal_paper_doi               10.1021/ic102430a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C59 H66 B3 F12 N11 Ni2 O12'
_chemical_formula_weight         1499.08
_space_group_IT_number           37
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      37
_symmetry_space_group_name_Hall  'C 2 -2c'
_symmetry_space_group_name_H-M   'C c c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                co_sh46
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.079(6)
_cell_length_b                   34.385(18)
_cell_length_c                   35.122(18)
_cell_measurement_reflns_used    8190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.25
_cell_volume                     13380(12)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            124490
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       needle
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'inversion twin 0.61(1):0.39(1)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         13689
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0595P)^2^+33.5701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                10835
_reflns_number_total             13689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102430a_si_002_5.cif
_cod_data_source_block           co_sh46_sq
_cod_original_cell_volume        13379(13)
_cod_database_code               4325724
_audit_block_refno               866