Facile Oxidation-Based Synthesis of Sterically Encumbered Four-Coordinate Bis(2,9-di-tert-butyl-1,10-phenanthroline)copper(I) and Related Three-Coordinate Copper(I) Complexes
Bhavesh A. Gandhi; Omar Green; Judith N. Burstyn; Inorganic Chemistry 46 (2007) 3816–3825; doi:10.1021/ic0615224

data_4307021
_publ_contact_author_address
;University of Wisconsin-Madison
Department of Chemistry
1101 University Ave
Madison, WI 53706
;
_publ_contact_author_email       burstyn@chem.wisc.edu
_publ_contact_author_fax         608-262-6143
_publ_contact_author_name        'Judith N. Burstyn'
_publ_contact_author_phone       608-262-0328
_publ_section_title
;
Facile Oxidation-Based Synthesis of Sterically Encumbered Four-Coordinate
Bis(2,9-di-tert-butyl-1,10-phenanthroline)copper(I) and Related
Three-Coordinate Copper(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3816
_journal_page_last               3825
_journal_paper_doi               10.1021/ic0615224
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C65 H50 B Cl2 Cu F20 N4'
_chemical_formula_weight         1412.34
_chemical_name_systematic
; 
 bis(2,9-di-tert-butyl-1,10-phenanthroline)copper(I) 
perfluorotetraphenylborate dichloromethane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.057(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7039(14)
_cell_length_b                   25.882(3)
_cell_length_c                   16.7036(16)
_cell_measurement_temperature    100(2)
_cell_volume                     6043.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49961
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.8731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS V.2.05, Bruker AXS(2000-2003))'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         12323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0596P)^2^+9.1395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                8720
_reflns_number_total             12323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0615224si20060811_013837.cif
_cod_data_source_block           dtp2CuBC24F20CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6043.8(10)
_cod_database_code               4307021