Diiodomethane as Halogen Bond Donor toward Metal-bound Halides
Novikov, Alexander S.; Ivanov, Daniil M.; Avdontceva, Margarita S.; Kukushkin, Vadim Yu.; CrystEngComm  (2017) –; doi:10.1039/C7CE00346C

data_7227974
_publ_section_title
;
 Diiodomethane as Halogen Bond Donor toward Metal-bound Halides
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00346C
_journal_year                    2017
_chemical_formula_moiety         'C26 H30 Cl N5 Pt, 0.5(C H2 I2)'
_chemical_formula_sum            'C26.5 H31 Cl I N5 Pt'
_chemical_formula_weight         777.00
_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
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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_audit_update_record
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2017-02-10 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                99.4445(18)
_cell_angle_beta                 93.0501(15)
_cell_angle_gamma                93.7936(17)
_cell_formula_units_Z            4
_cell_length_a                   10.8895(2)
_cell_length_b                   15.6795(4)
_cell_length_c                   16.3632(3)
_cell_measurement_reflns_used    18199
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.8110
_cell_measurement_theta_min      3.1180
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
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_diffrn_measured_fraction_theta_max 0.998
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  1 omega  -20.00   72.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -99.0000 -120.0000 92

  2 omega  -23.00   53.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -38.0000  -90.0000 76

  3 omega    1.00   27.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000    0.0000 26

  4 omega   42.00  106.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000    0.0000 64

  5 omega    7.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811 -132.0000   84.0000 84

  6 omega    9.00   92.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   57.0000 -180.0000 83

  7 omega   35.00   65.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  178.0000    0.0000 30

  8 omega  -44.00    4.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega    9.00   36.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -57.0000   90.0000 27

 10 omega   -2.00   37.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000  150.0000 39

 11 omega -117.00  -73.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.1623 -178.0000   30.0000 44

 12 omega    4.00   80.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   38.0000  -90.0000 76

 13 omega   -4.00  107.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   77.0000   60.0000 111

 14 omega    0.00   42.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   57.0000  -30.0000 42

 15 omega   52.00   81.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811   57.0000  -30.0000 29

 16 omega    4.00   51.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       29.8811  -19.0000   90.0000 47
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0336812000
_diffrn_orient_matrix_UB_12      0.0281583000
_diffrn_orient_matrix_UB_13      -0.0219511000
_diffrn_orient_matrix_UB_21      0.0255699000
_diffrn_orient_matrix_UB_22      0.0244317000
_diffrn_orient_matrix_UB_23      0.0381626000
_diffrn_orient_matrix_UB_31      0.0499121000
_diffrn_orient_matrix_UB_32      -0.0269347000
_diffrn_orient_matrix_UB_33      -0.0009811000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50780
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.044
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.176
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_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     634
_refine_ls_number_reflns         11374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9492
_reflns_number_total             11374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00346c2.cif
_cod_data_source_block           dan43ch2i2
_cod_depositor_comments
;

2017-11-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C53 H62 Cl2 I2 N10 Pt2'
_cod_original_formula_weight         1554.00
_cod_original_formula_moiety         '2(C26 H30 Cl N5 Pt), C H2 I2'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2744.15(10)
_cod_database_code               7227974
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C24 H32 N5 Pt1 Cl1I2'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.02
_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.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N1(H1), N5A(H5A), N1A(H1A), C18(H18), C11A(H11A), C22A(H22A),
 C22(H22), C15A(H15A), C19A(H19A), C14A(H14A), C13(H13), C14(H14), C18A(H18A),
 C19(H19), C13A(H13A), C15(H15), C11(H11), C12A(H12A), C21A(H21A), C21(H21),
 C12(H12), C20(H20), C20A(H20A)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C26(H26A,H26B,H26C), C7(H7A,H7B,H7C),
 C6A(H6AA,H6AB,H6AC), C24(H24A,H24B,H24C), C7A(H7AA,H7AB,H7AC), C25A(H25D,H25E,
 H25F), C25(H25A,H25B,H25C), C8A(H8AA,H8AB,H8AC), C24A(H24D,H24E,H24F),
 C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              57980
_olex2_submission_special_instructions 'No special instructions were received'