Influence of Second Coordination Sphere Hydroxyl Groups on the Reactivity of Copper(I) Complexes
Christopher S. Letko; Thomas B. Rauchfuss; Xiaoyuan Zhou; Danielle L. Gray; Inorganic Chemistry 51 (2012) 4511–4520; doi:10.1021/ic202207e

data_4328885
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       dgray@illinois.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Influence of Second Coordination Sphere Hydroxyl Groups on the Reactivity
 of Copper(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4511
_journal_page_last               4520
_journal_paper_doi               10.1021/ic202207e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C32 H12 B F24, 2 C H2 Cl2, C34 H26 Cu2 N6 O4'
_chemical_formula_sum            'C68 H42 B Cl4 Cu2 F24 N6 O4'
_chemical_formula_weight         1742.77
_chemical_name_systematic
; 
? 
;
_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
_audit_update_record
; 
? 
;
_cell_angle_alpha                110.5200(10)
_cell_angle_beta                 97.9040(10)
_cell_angle_gamma                106.5470(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1997(15)
_cell_length_b                   15.3184(16)
_cell_length_c                   18.6560(19)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.24
_cell_volume                     3513.5(6)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm77pasq
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53676
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.8691
_exptl_absorpt_correction_T_min  0.7599
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       prism
_exptl_crystal_F_000             1742
_exptl_crystal_id                bm77pasq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (2 -1 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.319
_platon_squeeze_details
; 
The electron count from the "squeeze" model is an underestimates 
of the electron count from the solvate molecules.  This could be 
because of the extreme disorder in the F atoms on the "BARF" 
counterion or because of partial occupancies of the solvate molecules. 
The electron count is more consistent with 2 DCM per unit cell and 
not the predicted 4 for the starting structure model. 
;
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         13017
_refine_ls_number_restraints     1239
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0366P)^2^+3.0161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                10878
_reflns_number_total             13017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202207e_si_002_6.cif
_cod_data_source_block           bm77pasq
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4328885