Supramolecular adducts based on weak interactions between the trimeric Lewis acid complex (perfluoro-ortho-phenylene)mercury and polypnictogen complexes.
Fleischmann, Martin; Jones, James S.; Balázs, Gábor; Gabbaï, François P; Scheer, Manfred; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13742–13749; doi:10.1039/c6dt02507b

data_7039981
_publ_section_title
;
 Supramolecular adducts based on weak interactions between the trimeric
 Lewis acid complex (perfluoro-ortho-phenylene)mercury and polypnictogen
 complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13742
_journal_page_last               13749
_journal_paper_doi               10.1039/c6dt02507b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C24 H15 Bi1 Mo3 O9'
_chemical_formula_sum            'C24 H15 Bi Mo3 O9'
_chemical_formula_weight         944.16
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.8747(6)
_cell_length_b                   14.8747(6)
_cell_length_c                   7.4995(4)
_cell_measurement_reflns_used    1647
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      22.9700
_cell_measurement_theta_min      4.1360
_cell_volume                     1437.01(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9702
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details
;
  1 omega  -20.00   43.00   0.2000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5716  -99.0000 -150.0000 315

  2 omega  -16.00   81.00   0.2000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5716   77.0000    0.0000 485

  3 omega  -18.00   33.00   0.2000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5716   77.0000 -180.0000 255

  4 omega  -20.00   53.00   0.2000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5716  -99.0000   30.0000 365
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0271605000
_diffrn_orient_matrix_UB_12      -0.0422947000
_diffrn_orient_matrix_UB_13      0.0593386000
_diffrn_orient_matrix_UB_21      -0.0304312000
_diffrn_orient_matrix_UB_22      0.0217087000
_diffrn_orient_matrix_UB_23      0.0293192000
_diffrn_orient_matrix_UB_31      -0.0369639000
_diffrn_orient_matrix_UB_32      -0.0277444000
_diffrn_orient_matrix_UB_33      -0.0676047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1451
_diffrn_reflns_av_unetI/netI     0.1541
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5998
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_min         3.143
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.429
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_preparation
'Reaction of BiCl3 with Na[CpMo(CO)3] in THF.'
_exptl_crystal_recrystallization_method 'Cooling a concentrated THF solution.'
_exptl_crystal_size_max          0.2659
_exptl_crystal_size_mid          0.0249
_exptl_crystal_size_min          0.0169
_refine_diff_density_max         2.324
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Flack x determined using 343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1680
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.791
_reflns_number_gt                986
_reflns_number_total             1680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02507b2.cif
_cod_data_source_block           mf270_brown_oct15
_cod_depositor_comments
'Adding full bibliography for 7039972--7039981.cif.'
_cod_original_cell_volume        1437.01(16)
_cod_database_code               7039981
_chemical_oxdiff_formula         Bi(MoC3O3C5H5)3
_reflns_odcompleteness_completeness 90.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'mineral oil'
_olex2_submission_original_sample_id MF270_brown
_olex2_submission_special_instructions 'No special instructions were received'