Diamondoid Hydrazones and Hydrazides: Sterically Demanding Ligands for Sn/S Cluster Design
Barth, Beatrix E. K.; Tkachenko, Boryslav A.; Eußner, Jens P.; Schreiner, Peter R.; Dehnen, Stefanie; Organometallics 33 (2014) 1678–; doi:10.1021/om500014z

data_4082940
_publ_section_title
;
 Diamondoid Hydrazones and Hydrazides: Sterically Demanding Ligands for
 Sn/S Cluster Design
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1678
_journal_paper_doi               10.1021/om500014z
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C68 H108 N8 O4 S10 Sn6, 3.5(C H2 Cl2)'
_chemical_formula_sum            'C71.5 H115 Cl7 N8 O4 S10 Sn6'
_chemical_formula_weight         2431.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.694(5)
_cell_angle_beta                 88.532(5)
_cell_angle_gamma                77.329(5)
_cell_formula_units_Z            4
_cell_length_a                   16.2629(10)
_cell_length_b                   20.5736(12)
_cell_length_c                   30.064(2)
_cell_measurement_temperature    100(2)
_cell_volume                     9754.6(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_av_sigmaI/netI    0.2547
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            76383
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    1.964
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.8575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4842
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2032
_refine_ls_number_reflns         34351
_refine_ls_number_restraints     299
_refine_ls_restrained_S_all      0.801
_refine_ls_R_factor_all          0.1936
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                12978
_reflns_number_total             34351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500014z_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments          'Adding full bibliography for 4082940.cif.'
_cod_original_cell_volume        9754.8(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C71.50 H115 Cl7 N8 O4 S10 Sn6'
_cod_database_code               4082940