Catalytic cyanosilylation using germylene stabilized platinum(ii) dicyanide.
Sharma, Mahendra Kumar; Singh, Dharmendra; Mahawar, Pritam; Yadav, Ravi; Nagendran, Selvarajan; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5943–5947; doi:10.1039/C8DT00043C

data_7045798
_publ_section_title
;
 Catalytic cyanosilylation using germylene stabilized platinum(ii)
 dicyanide.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5943
_journal_page_last               5947
_journal_paper_doi               10.1039/C8DT00043C
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C38 H60 Ge2 N6 Pt'
_chemical_formula_sum            'C38 H60 Ge2 N6 Pt'
_chemical_formula_weight         941.22
_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     iterative
_audit_creation_date             2017-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-11-14 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                72.036(2)
_cell_angle_beta                 80.201(2)
_cell_angle_gamma                75.546(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9108(16)
_cell_length_b                   12.3525(16)
_cell_length_c                   17.527(2)
_cell_measurement_reflns_used    2966
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.26
_cell_volume                     2363.2(5)
_computing_cell_refinement       'SAINT v6.28A (Bruker, 2002)'
_computing_data_reduction        'SAINT v6.28A (Bruker, 2002)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12332
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.032
_diffrn_reflns_theta_min         1.775
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_min  0.714604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.0552 before and 0.0347 after correction.
The Ratio of minimum to maximum transmission is 0.7146.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.529
_exptl_transmission_factor_min   0.445
_refine_diff_density_max         2.356
_refine_diff_density_min         -4.112
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.00048(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         8173
_refine_ls_number_restraints     373
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6362
_reflns_number_total             8173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00043c2.cif
_cod_data_source_block           msha27m
_cod_depositor_comments
'Adding full bibliography for 7045794--7045798.cif.'
_cod_database_code               7045798
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C17
 1.65 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) = Uanis(C18)
Uanis(C31) = Uanis(C32)
Uanis(C27) = Uanis(C31)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C32(H32), C28(H28), C13(H13), C9(H9), C35(H35), C16(H16)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C31(H31A,H31B), C8(H8A,H8B), C27(H27A,H27B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C21(H21), C2(H2), C5(H5), C4(H4), C23(H23), C3(H3), C22(H22),
 C25(H25), C24(H24)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C34(H34A,H34B,H34C), C29(H29A,H29B,H29C), C36(H36A,H36B,
 H36C), C10(H10A,H10B,H10C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C30(H30A,
 H30B,H30C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              93376
_shelx_fab_checksum              35679
_olex2_submission_special_instructions 'No special instructions were received'