Direct Cupration of Fluoroform
Alessandro Zanardi; Maxim A. Novikov; Eddy Martin; Jordi Benet-Buchholz; Vladimir V. Grushin; Journal of the American Chemical Society 133 (2011) 20901–20913; doi:10.1021/ja2081026

data_4107238
_publ_section_title
;
 Direct Cupration of Fluoroform
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20901
_journal_page_last               20913
_journal_paper_doi               10.1021/ja2081026
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C72 H164 Cu6 I2 K8 N8 O20'
_chemical_formula_weight         2409.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.754(2)
_cell_length_b                   17.754(2)
_cell_length_c                   62.184(7)
_cell_measurement_reflns_used    3069
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.98
_cell_measurement_theta_min      2.73
_cell_volume                     16975(3)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Apex DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Quazar MX multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            28860
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'Metal ceramics X-ray Tube MCMB 50-0.6b'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_type              'Microfocus Source E025 IuS'
_exptl_absorpt_coefficient_mu    2.003
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.556
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3220
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+114.7264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                2221
_reflns_number_total             3220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2081026_si_001_3.cif
_cod_data_source_block           3_mo_az0621_0m
_cod_original_cell_volume        16974(4)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4107238