Heteroleptic Silver(I) Complexes Prepared from Phenanthroline and Bis-phosphine Ligands
Adrien Kaeser; Béatrice Delavaux-Nicot; Carine Duhayon; Yannick Coppel; Jean-François Nierengarten; Inorganic Chemistry 52 (2013) 14343–14354; doi:10.1021/ic402342y

data_4337027
_publ_contact_author_address
; 
Laboratoire de Chimie de Coordination du CNRS
(UPR 8241), Universit\'e de Toulouse (UPS, INP), 
205 Route de Narbonne, 31077 Toulouse, France
;
_publ_contact_author_email       nierengarten@unistra.fr
_publ_contact_author_name        'Adrien Kaeser'
_publ_contact_author_phone       '+33 (0)3 68 85 27 63'
_publ_section_title
;
 Heteroleptic Silver(I) Complexes Prepared from Phenanthroline and
 Bis-phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14343
_journal_page_last               14354
_journal_paper_doi               10.1021/ic402342y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C54 H48 Ag2 P2 N4, 2(B F4), 23/6(H2 O) '
_chemical_formula_sum            'C54 H55.667 Ag2 B2 F8 N4 O3.833 P2'
_chemical_formula_weight         1273.35
_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
_audit_creation_date             06-10-13
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 94.628(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   37.9967(16)
_cell_length_b                   32.2079(13)
_cell_length_c                   14.0707(6)
_cell_measurement_reflns_used    9347
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     17163.5(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.072
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            155144
_diffrn_reflns_theta_full        29.021
_diffrn_reflns_theta_max         29.021
_diffrn_reflns_theta_min         2.684
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             7640
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.25
_refine_diff_density_min         -1.97
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         10882
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.2154
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          0.008425
_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: 
 13.1 12.5 11.8 4.80 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1121
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0902
_reflns_limit_h_max              51
_reflns_limit_h_min              -51
_reflns_limit_k_max              44
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                10882
_reflns_number_total             45818
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            ic402342y_si_006.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4337027