Synthesis of Small Tetranuclear Cu(I) Metallacycles Based on Bridging Pseudohalogenide Ions
Volodymyr Vreshch; Brigitte Nohra; Christophe Lescop; Régis Réau; Inorganic Chemistry 52 (2013) 1496–1503; doi:10.1021/ic3022535

data_4333715
_publ_section_title
;
 Synthesis of Small Tetranuclear Cu(I) Metallacycles Based on Bridging
 Pseudohalogenide Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1496
_journal_page_last               1503
_journal_paper_doi               10.1021/ic3022535
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_sum            'C98 H84 Cl0 Cu4 F12 N10 O0 P6'
_chemical_formula_weight         2069.73
_chemical_name_systematic
;
 ?
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-05-10T17:14:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.491(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3250(6)
_cell_length_b                   20.6150(11)
_cell_length_c                   18.4860(9)
_cell_measurement_reflns_used    7246
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     4993.1(4)
_computing_cell_refinement       'Bruker SMART, 2006'
_computing_data_collection       'Bruker SMART, 2006'
_computing_data_reduction        'Bruker SAINT, 2006'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by SAINT Bruker-AXS'
_diffrn_orient_matrix_UB_11      0.355782E-1
_diffrn_orient_matrix_UB_12      0.440057E-1
_diffrn_orient_matrix_UB_13      -0.252313E-1
_diffrn_orient_matrix_UB_21      -0.175094E-1
_diffrn_orient_matrix_UB_22      -0.270936E-1
_diffrn_orient_matrix_UB_23      -0.425413E-1
_diffrn_orient_matrix_UB_31      -0.664204E-1
_diffrn_orient_matrix_UB_32      0.182198E-1
_diffrn_orient_matrix_UB_33      -0.23401E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59447
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.08
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.9059
_exptl_absorpt_correction_T_min  0.5740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       prism
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         3.971
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10063
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+9.5541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1811
_reflns_number_gt                8345
_reflns_number_total             10063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3022535_si_002_1.cif
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4333715