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_4082941
_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
'C52 H84 N8 O4 S10 Sn6, 2(C4 H8 O2), 4(C H Cl3)'
_chemical_formula_sum            'C64 H104 Cl12 N8 O8 S10 Sn6'
_chemical_formula_weight         2571.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.732(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7197(7)
_cell_length_b                   30.9148(10)
_cell_length_c                   11.1030(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4641.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  IPDS2T
_diffrn_measurement_method       /w
_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  0.1409
_diffrn_reflns_av_sigmaI/netI    0.1216
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            42698
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    2.212
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XPREP in SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                4130
_reflns_number_total             8180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500014z_si_002.cif
_cod_data_source_block           compound9a
_cod_depositor_comments          'Adding full bibliography for 4082941.cif.'
_cod_original_cell_volume        4641.5(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4082941