A family of heterotetrameric clusters of chloride species and halomethanes held by two halogen and two hydrogen bonds
Ivanov, Daniil M.; Novikov, Alexander S.; Starova, Galina L.; Haukka, Matti; Kukushkin, Vadim Yu.; CrystEngComm 18 (2016) 5278–; doi:10.1039/C6CE01179A

data_7225554
_publ_section_title
;
 A family of heterotetrameric clusters of chloride species and
 halomethanes held by two halogen and two hydrogen bonds
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5278
_journal_paper_doi               10.1039/C6CE01179A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '4(C26 H30 Cl N5 Pt), 5.5(C H2 Cl2)'
_chemical_formula_sum            'C109.5 H131 Cl15 N20 Pt4'
_chemical_formula_weight         3039.45
_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_block_doi                 10.5517/ccdc.csd.cc1lby3z
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-23 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.512(3)
_cell_angle_beta                 87.526(2)
_cell_angle_gamma                85.480(2)
_cell_formula_units_Z            1
_cell_length_a                   10.7179(3)
_cell_length_b                   13.6861(4)
_cell_length_c                   20.5784(7)
_cell_measurement_reflns_used    11654
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2437
_cell_measurement_theta_min      2.5948
_cell_volume                     2993.46(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details
;
  1 omega  -22.00    3.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000  -30.0000 25

  2 omega  -12.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000 -120.0000 36

  3 omega  -89.00  -36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777 -178.0000  -60.0000 53

  4 omega  -24.00   10.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000   60.0000 34

  5 omega  -53.00    7.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -38.0000    0.0000 60

  6 omega   13.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -38.0000    0.0000 31

  7 omega  -53.00   37.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -38.0000  -90.0000 90

  8 omega  -50.00  -25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -77.0000  150.0000 25

  9 omega   37.00   66.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  178.0000 -150.0000 29

 10 omega  -17.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  -77.0000  150.0000 66

 11 omega   22.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714   57.0000 -120.0000 64

 12 omega  -27.00    0.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  119.0000 -126.0000 27

 13 omega  -71.00  -31.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  119.0000 -126.0000 40

 14 omega   35.00   71.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714  178.0000  -60.0000 36

 15 omega    5.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714   57.0000  -30.0000 83

 16 omega   -2.00   48.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9714   57.0000 -180.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0032232000
_diffrn_orient_matrix_UB_12      -0.0059247000
_diffrn_orient_matrix_UB_13      -0.0337394000
_diffrn_orient_matrix_UB_21      -0.0136334000
_diffrn_orient_matrix_UB_22      0.0514662000
_diffrn_orient_matrix_UB_23      -0.0065923000
_diffrn_orient_matrix_UB_31      0.0649340000
_diffrn_orient_matrix_UB_32      0.0065006000
_diffrn_orient_matrix_UB_33      -0.0043315000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45118
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.308
_diffrn_reflns_theta_min         2.600
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       needle
_exptl_crystal_F_000             1495
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.876
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         14233
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0240P)^2^+18.8200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11358
_reflns_number_total             14233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01179a2.cif
_cod_data_source_block           dan
_cod_depositor_comments
'Adding full bibliography for 7225552--7225554.cif.'
_cod_original_cell_volume        2993.47(15)
_cod_original_formula_sum        'C109.50 H131 Cl15 N20 Pt4'
_cod_database_code               7225554
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'pt1 o8 c2 h10 cl2'
_reflns_odcompleteness_completeness 99.89
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4S-C2S = Cl3S-C2S = Cl4S-C3S = Cl3S-C3S
 1.77 with sigma of 0.02
 Cl3S-C3S = Cl4S-C3S = Cl4S-C2S = Cl3S-C2S
 1.77 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3S) = Uanis(C2S)
Uanis(C6) = Uanis(C7) = Uanis(C8)
4. Others
 Fixed Sof: Cl3S(0.75) Cl4S(0.75) C2S(0.45) H2SA(0.45) H2SB(0.45) C3S(0.3)
 H3SA(0.3) H3SB(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C4S(H4SA,H4SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Aromatic/amide H refined with riding coordinates:
 N5A(H5A), N5(H5), N1A(H1A), N1(H1), C14A(H14A), C11(H11), C15A(H15A),
 C22(H22), C19(H19), C13(H13), C15(H15), C13A(H13A), C22A(H22A), C18(H18),
 C11A(H11A), C14(H14), C12A(H12A), C21A(H21A), C18A(H18A), C19A(H19A), C21(H21),
  C12(H12), C20(H20), C20A(H20A)
5.c Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C6(H6A,H6B,H6C), C24(H24D,H24E,H24F), C7A(H7AA,H7AB,
 H7AC), C8A(H8AA,H8AB,H8AC), C8(H8A,H8B,H8C), C24A(H24A,H24B,H24C), C7(H7A,H7B,
 H7C), C26A(H26A,H26B,H26C), C26(H26D,H26E,H26F), C25A(H25A,H25B,H25C),
 C25(H25D,H25E,H25F)
;
_shelx_res_checksum              95660
_olex2_submission_special_instructions 'No special instructions were received'