Cu(I) Complexes of 3,3'-Polymethylene Bridged Derivatives of 2,2'-Bi-1,10-Phenanthroline
Elvira C. Riesgo; Yi-Zhen Hu; Randolph P. Thummel; Inorganic Chemistry 42 (2003) 6648–6654; doi:10.1021/ic0300417

data_4312303
_publ_section_title
;
 Cu(I) Complexes of 3,3'-Polymethylene Bridged Derivatives of
 2,2'-Bi-1,10-Phenanthroline
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6648
_journal_page_last               6654
_journal_paper_doi               10.1021/ic0300417
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C52 H32 N8 Cu2 2+, 2 P F6 -, 4 C2 H3 N'
_chemical_formula_sum            'C60 H44 Cu2 F12 N12 P2'
_chemical_formula_weight         1350.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            8
_cell_length_a                   19.9779(13)
_cell_length_b                   22.2432(14)
_cell_length_c                   25.9316(17)
_cell_measurement_reflns_used    5624
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.41
_cell_volume                     11523.3(13)
_computing_cell_refinement       'Bruker SAINT software (Bruker, 1999)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12272
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.2808
_exptl_absorpt_correction_T_min  0.4455
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Very dark olive green'
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00011(5)
_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   1.217
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2059
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+186.3518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1966
_reflns_number_gt                1550
_reflns_number_total             2254
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic0300417.cif
_cod_data_source_block           ic0300417.cif
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C60 H44 F12 N12 P2 Cu2'
_cod_database_code               4312303