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_7039975
_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 Mo2 O4 Sb2, C18 F12 Hg3, C H2 Cl2'
_chemical_formula_sum            'C33 H12 Cl2 F12 Hg3 Mo2 O4 Sb2'
_chemical_formula_weight         1808.48
_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                81.649(2)
_cell_angle_beta                 71.018(2)
_cell_angle_gamma                63.354(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4435(3)
_cell_length_b                   13.3321(3)
_cell_length_c                   14.0134(4)
_cell_measurement_reflns_used    7051
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      28.7690
_cell_measurement_theta_min      3.1030
_cell_volume                     1964.89(10)
_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)
;
_computing_data_reduction
;
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      123.00(14)
_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 0.998
_diffrn_measurement_details
;
  1 omega  -86.00    8.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.8018  -57.0000  120.0000 188

  2 omega  -15.00   81.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   77.0000   30.0000 192

  3 omega   60.00   88.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   57.0000 -180.0000 56

  4 omega   57.00   82.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  178.0000   90.0000 50

  5 omega  -38.00  -12.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  -57.0000   90.0000 52

  6 omega  -64.00   41.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955  -77.0000  -90.0000 210

  7 omega  -14.00   11.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8955   57.0000 -180.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0345794000
_diffrn_orient_matrix_UB_12      -0.0572804000
_diffrn_orient_matrix_UB_13      0.0103568000
_diffrn_orient_matrix_UB_21      -0.0154320000
_diffrn_orient_matrix_UB_22      -0.0161788000
_diffrn_orient_matrix_UB_23      -0.0379481000
_diffrn_orient_matrix_UB_31      0.0549412000
_diffrn_orient_matrix_UB_32      0.0005045000
_diffrn_orient_matrix_UB_33      -0.0362996000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19426
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.877
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.331
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.057
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_recrystallization_method 'Crystallization from DCM.'
_exptl_crystal_size_max          0.1217
_exptl_crystal_size_mid          0.0843
_exptl_crystal_size_min          0.0394
_refine_diff_density_max         2.144
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8644
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0149P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5727
_reflns_number_total             8644
_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        1964.90(9)
_cod_database_code               7039975
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Hg3F12Cl2Mo2Sb2O4C33H12
_reflns_odcompleteness_completeness 99.85
_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. Restrained distances
 C33-Cl1 \\sim C33-Cl2 \\sim C34-Cl3 \\sim C34-Cl4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: C33(0.62) H33A(0.62) H33B(0.62) Cl1(0.62) Cl2(0.62) C34(0.38)
 H34A(0.38) H34B(0.38) Cl3(0.38) Cl4(0.38)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B)
5.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 MF179_orangeblock
_olex2_submission_special_instructions 'No special instructions were received'