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_7039976
_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         'C46 H20 Bi4 F12 Hg3 Mo4 O8, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H24 Bi4 Cl4 F12 Hg3 Mo4 O8'
_chemical_formula_weight         2919.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                111.087(2)
_cell_angle_beta                 103.308(2)
_cell_angle_gamma                104.4830(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5154(2)
_cell_length_b                   14.6000(2)
_cell_length_c                   17.6515(3)
_cell_measurement_reflns_used    23860
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      29.7210
_cell_measurement_theta_min      2.9410
_cell_volume                     2942.32(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
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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_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5431
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -40.00    4.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018   19.0000  -60.0000 88

  2 omega  -80.00   17.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018  -57.0000   90.0000 194

  3 omega   36.00   62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018   19.0000  -60.0000 52

  4 omega   42.00   77.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   77.0000  150.0000 70

  5 omega  -11.00   82.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   57.0000   30.0000 186

  6 omega  -14.00   16.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   77.0000  150.0000 60

  7 omega  -56.00   40.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  -57.0000 -120.0000 192

  8 omega  -39.00   63.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018   38.0000   90.0000 204

  9 omega -103.00  -35.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018 -178.0000 -150.0000 136

 10 omega  -87.00   17.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018  -57.0000  -60.0000 208

 11 omega   57.00  104.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  178.0000  -90.0000 94

 12 omega   -4.00   56.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  -99.0000 -180.0000 120

 13 omega  -13.00   90.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   38.0000  -90.0000 206

 14 omega  -60.00   -8.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  -57.0000 -120.0000 104

 15 omega    9.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955 -114.0000   69.0000 110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0346490000
_diffrn_orient_matrix_UB_12      -0.0212965000
_diffrn_orient_matrix_UB_13      -0.0193857000
_diffrn_orient_matrix_UB_21      0.0329786000
_diffrn_orient_matrix_UB_22      0.0076206000
_diffrn_orient_matrix_UB_23      0.0409782000
_diffrn_orient_matrix_UB_31      -0.0327404000
_diffrn_orient_matrix_UB_32      -0.0511930000
_diffrn_orient_matrix_UB_33      -0.0081390000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.705
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.797
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.203
_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            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.296
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_recrystallization_method 'Crystallization from DCM.'
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.0807
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         12972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0134P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9609
_reflns_number_total             12972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02507b2.cif
_cod_data_source_block           abs2
_cod_depositor_comments
'Adding full bibliography for 7039972--7039981.cif.'
_cod_original_cell_volume        2942.32(9)
_cod_database_code               7039976
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Hg3C18F12(Mo2Bi2C14O4H10)2(CH2Cl2)2
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C48(H48A,H48B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26)
;
_olex2_exptl_crystal_mounting_method 'mineral oil'
_olex2_submission_original_sample_id MF272_3F_2
_olex2_submission_special_instructions 'No special instructions were received'