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_7039974
_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         'C14 H10 As2 Mo2 O4, C18 F12 Hg3, C H2 Cl2'
_chemical_formula_sum            'C33 H12 As2 Cl2 F12 Hg3 Mo2 O4'
_chemical_formula_weight         1714.82
_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                60.580(3)
_cell_angle_beta                 71.346(3)
_cell_angle_gamma                69.203(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7941(3)
_cell_length_b                   13.4465(4)
_cell_length_c                   13.5405(5)
_cell_measurement_reflns_used    7610
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      29.4160
_cell_measurement_theta_min      3.1780
_cell_volume                     1866.34(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_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9702
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details
;
  1 omega    8.00   88.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2461   57.0000  -90.0000 160

  2 omega   42.00   80.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2461 -130.0000 -155.0000 76

  3 omega  -11.00   88.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2461   77.0000   30.0000 198

  4 omega  -18.00   89.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.2461   19.0000 -150.0000 214

  5 omega  -95.00  -70.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586 -178.0000  -30.0000 50

  6 omega  -95.00  -45.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586 -178.0000  120.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0299584000
_diffrn_orient_matrix_UB_12      0.0436253000
_diffrn_orient_matrix_UB_13      -0.0410660000
_diffrn_orient_matrix_UB_21      -0.0522633000
_diffrn_orient_matrix_UB_22      0.0427306000
_diffrn_orient_matrix_UB_23      -0.0093129000
_diffrn_orient_matrix_UB_31      0.0019296000
_diffrn_orient_matrix_UB_32      0.0127295000
_diffrn_orient_matrix_UB_33      0.0443019000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16291
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.655
_diffrn_reflns_theta_min         3.030
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.952
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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)
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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.051
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_recrystallization_method 'crystallization from DCM.'
_exptl_crystal_size_max          0.0752
_exptl_crystal_size_mid          0.0363
_exptl_crystal_size_min          0.0218
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0099P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0400
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6482
_reflns_number_total             8975
_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        1866.34(12)
_cod_database_code               7039974
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Hg3F12Cl2Mo2As2O4C33H12
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
;
_olex2_exptl_crystal_mounting_method 'mineral oil'
_olex2_submission_original_sample_id MF185
_olex2_submission_special_instructions 'No special instructions were received'