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_4307023
_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            'C40 H48 Cu F6 N4 Sb'
_chemical_formula_weight         884.11
_chemical_name_systematic
; 
 bis(2,9-di-tert-butyl-1,10-phenanthroline)copper(I) hexafluoroantimonate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.8330(10)
_cell_angle_beta                 109.7370(10)
_cell_angle_gamma                107.8140(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1995(5)
_cell_length_b                   13.6275(6)
_cell_length_c                   14.4027(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2114.31(16)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17554
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.8794
_exptl_absorpt_correction_T_min  0.8131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS V.2.05, Bruker AXS(2004))'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0438P)^2^+0.5324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                7122
_reflns_number_total             8527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0615224si20060811_013930.cif
_cod_data_source_block           dtp2CuBC24F20
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        2114.31(15)
_cod_database_code               4307023