Coupling of platinated triguanides with platinum-activated nitriles as a novel strategy for generation of dimetallic systems.
Serebryanskaya, Tatiyana V.; Novikov, Alexander S.; Gushchin, Pavel V.; Zolotarev, Andrey A.; Gurzhiy, Vladislav V.; Kukushkin, Vadim Yu; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6003–6011; doi:10.1039/c4dt03870c

data_7033998
_publ_section_title
;
 Coupling of platinated triguanides with platinum-activated nitriles as a
 novel strategy for generation of dimetallic systems.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6003
_journal_page_last               6011
_journal_paper_doi               10.1039/c4dt03870c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H33 Cl4 N9 Pt2, C0.13 H0.25 Cl0.25'
_chemical_formula_sum            'C24.12 H33.25 Cl4.25 N9 Pt2'
_chemical_formula_weight         990.19
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2015-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2015-01-13 deposited with the CCDC.
2015-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.753(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.9496(14)
_cell_length_b                   15.7777(5)
_cell_length_c                   17.6434(6)
_cell_measurement_reflns_used    9008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.5250
_cell_measurement_theta_min      2.7980
_cell_volume                     8190.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -48.00   46.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   77.0000 -180.0000 94

  2 omega   16.00   48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   77.0000 -150.0000 32

  3 omega  -48.00   29.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   77.0000   90.0000 77

  4 omega   22.00   48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777   77.0000  -60.0000 26

  5 omega   -9.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   77.0000   60.0000 45

  6 omega  -11.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   77.0000  -60.0000 94

  7 omega  -79.00    4.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -57.0000  150.0000 83

  8 omega    2.00   40.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777    0.0000 -180.0000 38

  9 omega  -82.00   -1.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -57.0000   60.0000 81

 10 omega  -77.00  -36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777    0.0000 -180.0000 41

 11 omega  -20.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -99.0000   30.0000 81

 12 omega  -20.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -99.0000  -60.0000 81
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0218330000
_diffrn_orient_matrix_UB_12      0.0026072000
_diffrn_orient_matrix_UB_13      0.0442380000
_diffrn_orient_matrix_UB_21      -0.0035348000
_diffrn_orient_matrix_UB_22      0.0430986000
_diffrn_orient_matrix_UB_23      0.0183140000
_diffrn_orient_matrix_UB_31      -0.0459670000
_diffrn_orient_matrix_UB_32      -0.0127515000
_diffrn_orient_matrix_UB_33      -0.0056812000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62905
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.582
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       prism
_exptl_crystal_F_000             3754
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The unit cell contains disordered dichloromethane 
molecules which have been treated as a diffuse
contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.576
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+12.9467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5721
_reflns_number_total             9356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03870c2.cif
_cod_data_source_block           3a_CCDC_1003611
_cod_depositor_comments
'Adding full bibliography for 7033998--7033999.cif.'
_cod_database_code               7033998
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.91
_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
 N1-C1
 1.3 with sigma of 0.02
 C1-C2
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(Cl5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.05
Uanis(Cl2A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.06
Uanis(C2) = Uanis(C1) = Uanis(N1)
Uanis(Cl5) = Uanis(C25)
Uanis(Cl2A) = Uanis(Cl2B)
4. Others
 Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2B)=FVAR(1)
 Fixed Sof: Cl5(0.25) C25(0.125) H25A(0.125) H25B(0.125)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C25(H25A,H25B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C)
;