Syntheses of a Novel Fluorinated Trisphosphinoborate Ligand and Its Copper and Silver Complexes. Catalytic Activity toward Nitrene Transfer Reactions.
Arenas, Ismael; Fuentes, M Ángeles; Alvarez, Eleuterio; Díaz, Yolanda; Caballero, Ana; Castillón, Sergio; Pérez, Pedro J; Inorganic chemistry 53 (2014) 3991–3999; doi:10.1021/ic4028223

data_4338069
_publ_section_title
;
 Syntheses of a Novel Fluorinated Trisphosphinoborate Ligand and Its
 Copper and Silver Complexes. Catalytic Activity toward Nitrene Transfer
 Reactions.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3991
_journal_page_last               3999
_journal_paper_doi               10.1021/ic4028223
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C69 H50 B Cu F18 P4, C4 H8 O'
_chemical_formula_sum            'C73 H58 B Cu F18 O P4'
_chemical_formula_weight         1491.42
_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
_cell_angle_alpha                78.198(2)
_cell_angle_beta                 77.615(2)
_cell_angle_gamma                88.162(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3419(5)
_cell_length_b                   13.1615(6)
_cell_length_c                   23.6682(11)
_cell_measurement_reflns_used    5808
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.33
_cell_measurement_theta_min      2.21
_cell_volume                     3377.7(3)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            88542
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.8815
_exptl_absorpt_correction_T_min  0.8420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 APEX2 Software Suite; Bruker 2005.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         20486
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+3.2792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                11463
_reflns_number_total             20486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4028223_si_002.cif
_cod_data_source_block           ea18212a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338069--4338071.cif.
;
_cod_database_code               4338069