Intermetallic Interactions in Face-to-Face Homo- and Heterodinuclear Bismacrocyclic Complexes of Copper(II) and Nickel(II)
Agnieszka Więckowska; Renata Bilewicz; Sławomir Domagała; Krzysztof Woźniak; Bohdan Korybut-Daszkiewicz; Alina Tomkiewicz; Jerzy Mroziński; Inorganic Chemistry 42 (2003) 5513–5522; doi:10.1021/ic034127b

data_4314150
_publ_contact_author_address
;  Chemistry Department,
Warsaw University,
Pasteura 1,
02-093 Warszawa,
Poland
;
_publ_contact_author_email       kwozniak@chem.uw.edu.pl
_publ_contact_author_fax         '48(22)8220211 ext. 212'
_publ_contact_author_name        'Prof. Krzysztof Wozniak'
_publ_contact_author_phone       48(22)8222892
_publ_section_title
;
 Intermetallic Interactions in Face-to-Face Homo- and Heterodinuclear
 Bismacrocyclic Complexes of Copper(II) and Nickel(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5513
_journal_page_last               5522
_journal_paper_doi               10.1021/ic034127b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C30 H44 Cu F24 N12 Ni O2 P4'
_chemical_formula_weight         1306.90
_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   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                   14.218(3)
_cell_length_b                   18.236(4)
_cell_length_c                   18.380(4)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     4765.6(18)
_computing_cell_refinement       CrysAlisRED
_computing_data_collection       CrysAlisCCD
_computing_data_reduction        CrysAlisRED
_computing_molecular_graphics    Diamond
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 1024
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'omega scan'
_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  0.2421
_diffrn_reflns_av_sigmaI/netI    0.2780
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25434
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count '50 frames'
_diffrn_standards_number         '1 frame'
_exptl_absorpt_coefficient_mu    1.116
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(8)
_refine_ls_extinction_coef       0.00000(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1851
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          5.127
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                2017
_reflns_number_total             5108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034127bsi20030205_013144_1.cif
_cod_data_source_block           3CuNi
_cod_original_cell_volume        4765.6(16)
_cod_database_code               4314150