Face-to-Face Dinuclear Scaffolds Composed of Tetraazamacrocyclic Charged and Neutral Complexes
Katarzyna Szczepaniak; Urszula E. Wawrzyniak; Jarosław Kowalski; Iwona Mames; Renata Bilewicz; Przemysław Kalicki; Bohdan Korybut-Daszkiewicz; Inorganic Chemistry 49 (2010) 4491–4498; doi:10.1021/ic902424z

data_4315557
_publ_section_title
;
 Face-to-Face Dinuclear Scaffolds Composed of Tetraazamacrocyclic Charged
 and Neutral Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4491
_journal_page_last               4498
_journal_paper_doi               10.1021/ic902424z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C34 H48 N10 Ni2 O4, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C36 H51 F12 N11 Ni2 O4 P2'
_chemical_formula_weight         1109.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.860(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8962(15)
_cell_length_b                   26.681(6)
_cell_length_c                   21.615(4)
_cell_measurement_reflns_used    1737
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      45.19
_cell_measurement_theta_min      3.89
_cell_volume                     4553.3(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1634
_diffrn_reflns_av_sigmaI/netI    0.1187
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30408
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         3.89
_exptl_absorpt_coefficient_mu    2.604
_exptl_absorpt_correction_T_max  0.8347
_exptl_absorpt_correction_T_min  0.4466
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00024(6)
_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   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         7881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1538
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                3716
_reflns_number_total             8047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902424z_si_001_1.cif
_cod_data_source_block           7Ni-n-Ni-ch
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4553.4(15)
_cod_database_code               4315557