Mixed guanidinato-amido Ge(IV) and Sn(IV) complexes with Ge=E (E = S, Se) double bond and SnS4, Sn2Se2 rings†
Barman, Milan Kumar; Nembenna, Sharanappa; RSC Adv.  (2015) –; doi:10.1039/C5RA24280K

data_7223495
_publ_section_title
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 Mixed guanidinato-amido Ge(IV) and Sn(IV) complexes with Ge=E (E = S, Se)
 double bond and SnS4, Sn2Se2 rings&#x2020;
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_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA24280K
_journal_year                    2015
_chemical_formula_moiety         'C29 H50 Ge N4 Se Si2'
_chemical_formula_sum            'C29 H50 Ge N4 Se Si2'
_chemical_formula_weight         662.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_audit_update_record
;
2015-11-11 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.622(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6303(10)
_cell_length_b                   10.2343(5)
_cell_length_c                   18.6276(9)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.43
_cell_volume                     3551.5(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.186
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0696 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.8043.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.717
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6983
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+5.7714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5817
_reflns_number_total             6983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra24280k2.cif
_cod_data_source_block           sn_mb_final
_cod_database_code               7223495
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C5(H5), C14(H14), C12(H12), C13(H13)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C),
 C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C27(H27A,
 H27B,H27C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              387
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'