Heteroleptic Copper(I) Complexes Prepared from Phenanthroline and Bis-Phosphine Ligands
Adrien Kaeser; Meera Mohankumar; John Mohanraj; Filippo Monti; Michel Holler; Juan-José Cid; Omar Moudam; Iwona Nierengarten; Lydia Karmazin-Brelot; Carine Duhayon; Béatrice Delavaux-Nicot; Nicola Armaroli; Jean-François Nierengarten; Inorganic Chemistry 52 (2013) 12140–12151; doi:10.1021/ic4020042

data_4336477
_publ_contact_author_address
; 
Laboratoire de Chimie des Mat\'eriaux Mol\'eculaires, 
Universit\'e de Strasbourg et CNRS (UMR 7509), 
25 rue Becquerel, 67087 Strasbourg Cedex 2, France
;
_publ_contact_author_email       nierengarten@unistra.fr
_publ_contact_author_name        'Jean-Francois Nierengarten'
_publ_contact_author_phone       '+33 (0)3 68 85 27 63'
_publ_section_title
;
 Heteroleptic Copper(I) Complexes Prepared from Phenanthroline and
 Bis-Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12140
_journal_page_last               12151
_journal_paper_doi               10.1021/ic4020042
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C72 H56 Cu O2 P4, B F4'
_chemical_formula_sum            'C72 H56 B Cu F4 O2 P4'
_chemical_formula_weight         1227.48
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-09-11
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0837(6)
_cell_length_b                   24.4373(7)
_cell_length_c                   24.7392(8)
_cell_measurement_reflns_used    8956
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     12141.8(6)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            116293
_diffrn_reflns_theta_full        29.082
_diffrn_reflns_theta_max         29.082
_diffrn_reflns_theta_min         2.612
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.52
_refine_diff_density_min         -1.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.000370
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 8.06 -1.62 6.05 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1085
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0761
_reflns_limit_h_max              27
_reflns_limit_h_min              0
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                6792
_reflns_number_total             16153
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            ic4020042_si_004.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C72 H56 B1 Cu1 F4 O2 P4'
_cod_database_code               4336477