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_4338071
_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         '4(C51 H35 B F18 P3 Tl), 3(C H2 Cl2)'
_chemical_formula_sum            'C207 H146 B4 Cl6 F72 P12 Tl4'
_chemical_formula_weight         5446.30
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.431(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6917(11)
_cell_length_b                   36.911(3)
_cell_length_c                   22.944(2)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.31
_cell_volume                     11365.3(16)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0662
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            116761
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  0.6895
_exptl_absorpt_correction_T_min  0.3419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 APEX2 Software Suite; Bruker 2005.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5324
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
;
_refine_diff_density_max         2.205
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1378
_refine_ls_number_reflns         19704
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+21.2443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                15476
_reflns_number_total             19704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4028223_si_004.cif
_cod_data_source_block           ea19012a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4338071