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_7039978
_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(C18 F12 Hg3), C20 H20 As5 Cr4, 3(C H2 Cl2)'
_chemical_formula_sum            'C59 H26 As5 Cl6 Cr4 F24 Hg6'
_chemical_formula_weight         3189.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 99.0540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.18520(10)
_cell_length_b                   19.78690(10)
_cell_length_c                   18.72880(10)
_cell_measurement_reflns_used    14637
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.3990
_cell_measurement_theta_min      3.7640
_cell_volume                     7021.16(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega   79.00  117.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5681   86.0000  -60.0000 76

  2 omega    0.00   96.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5681 -125.0000   60.0000 192

  3 omega  -21.00   46.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5681  -57.0000 -180.0000 134

  4 omega  130.00  156.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 52

  5 omega   94.00  131.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000 -162.0000 74

  6 omega   27.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 100

  7 omega   10.00   81.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -120.0000 142

  8 omega   16.00   48.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 64

  9 omega   39.00   81.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000    0.0000 84

 10 omega    9.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000 -162.0000 104

 11 omega   43.00   69.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -30.0000 52

 12 omega   17.00   43.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   60.0000 52

 13 omega   53.00   79.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   60.0000 52

 14 omega   35.00   88.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   30.0000 106

 15 omega   62.00  125.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 126

 16 omega   71.00  113.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -30.0000 84

 17 omega  125.00  160.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -30.0000 70

 18 omega   34.00   70.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 72

 19 omega   16.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -90.0000 90

 20 omega   42.00  119.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   60.0000 154

 21 omega -116.00  -27.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5681  -57.0000  120.0000 178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0492605000
_diffrn_orient_matrix_UB_12      -0.0335008000
_diffrn_orient_matrix_UB_13      -0.0471296000
_diffrn_orient_matrix_UB_21      -0.0097539000
_diffrn_orient_matrix_UB_22      0.0609102000
_diffrn_orient_matrix_UB_23      -0.0518547000
_diffrn_orient_matrix_UB_31      0.0639567000
_diffrn_orient_matrix_UB_32      0.0350279000
_diffrn_orient_matrix_UB_33      0.0450599000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21971
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        66.545
_diffrn_reflns_theta_max         67.679
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    33.451
_exptl_absorpt_correction_T_max  0.340
_exptl_absorpt_correction_T_min  0.030
_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 green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.017
_exptl_crystal_description       prism
_exptl_crystal_F_000             5756
_exptl_crystal_recrystallization_method 'Crystallization from DCM.'
_exptl_crystal_size_max          0.2399
_exptl_crystal_size_mid          0.0808
_exptl_crystal_size_min          0.0495
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0370P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5652
_reflns_number_total             6190
_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_database_code               7039978
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Hg6F24Cr4Cl6As5C59H26
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl4(0.5) C30(0.5) H30A(0.5) H30B(0.5) Cl3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C20(H20), C19(H19), C22(H22), C27(H27), C28(H28), C21(H21),
 C23(H23), C24(H24), C26(H26)
;
_olex2_exptl_crystal_mounting_method 'mineral oil'
_olex2_submission_original_sample_id MF146
_olex2_submission_special_instructions 'No special instructions were received'