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_7039973
_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
'2(C14 H10 Mo2 O4 P2), 2(C18 F12 Hg3), 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H24 Cl4 F24 Hg6 Mo4 O8 P4'
_chemical_formula_weight         3253.83
_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                92.367(4)
_cell_angle_beta                 100.819(4)
_cell_angle_gamma                94.276(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8301(7)
_cell_length_b                   12.8847(6)
_cell_length_c                   23.5633(12)
_cell_measurement_reflns_used    15018
_cell_measurement_temperature    123.1(5)
_cell_measurement_theta_max      30.1192
_cell_measurement_theta_min      2.8195
_cell_volume                     3809.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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(5)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega  -79.00    7.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.9580  -77.0000  150.0000 172

  2 omega  -10.00   83.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0518   57.0000   60.0000 186

  3 omega  -53.00   35.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0518  -57.0000  -90.0000 176

  4 omega -103.00  -35.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.9580 -178.0000 -120.0000 136

  5 omega  -39.00   63.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.9580   38.0000  120.0000 204

  6 omega  -92.00    6.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.9580  -77.0000    0.0000 196

  7 omega   53.00  102.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0518 -178.0000  -60.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0156997000
_diffrn_orient_matrix_UB_12      -0.0207168000
_diffrn_orient_matrix_UB_13      -0.0251610000
_diffrn_orient_matrix_UB_21      0.0454425000
_diffrn_orient_matrix_UB_22      0.0364433000
_diffrn_orient_matrix_UB_23      0.0050017000
_diffrn_orient_matrix_UB_31      0.0296463000
_diffrn_orient_matrix_UB_32      -0.0360537000
_diffrn_orient_matrix_UB_33      0.0168558000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.186
_diffrn_reflns_theta_min         2.825
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.011
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_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    2.837
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_preparation       'mineral oil'
_exptl_crystal_recrystallization_method 'crystallization from DCM'
_exptl_crystal_size_max          0.1737
_exptl_crystal_size_mid          0.1183
_exptl_crystal_size_min          0.0574
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         19714
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17514
_reflns_number_total             19714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02507b2.cif
_cod_data_source_block           abs
_cod_depositor_comments
'Adding full bibliography for 7039972--7039981.cif.'
_cod_database_code               7039973
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Mo2P2O4Hg3F12C33H12Cl2
_reflns_odcompleteness_completeness 99.72
_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
 C65-Cl1 \\sim C65-Cl2 \\sim C67-Cl5 \\sim C67-Cl6
 with sigma of 0.02
 C66-Cl3 \\sim C66-Cl4 \\sim C68-Cl7 \\sim C68-Cl8
 with sigma of 0.02
3. Others
 Fixed Sof: C65(0.69) H65A(0.69) H65B(0.69) Cl1(0.69) Cl2(0.69) C67(0.31)
 H67A(0.31) H67B(0.31) Cl5(0.31) Cl6(0.31) C66(0.74) H66A(0.74) H66B(0.74)
 Cl3(0.74) Cl4(0.74) C68(0.26) H68A(0.26) H68B(0.26) Cl7(0.26) Cl8(0.26)
4.a Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C67(H67A,H67B), C66(H66A,H66B), C68(H68A,H68B)
4.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 MF136
_olex2_submission_special_instructions 'No special instructions were received'