An Efficient Route for the Synthesis of a Tin(II) Substituted Carbodiimide from a Diazo Compound
Anukul Jana; Herbert W. Roesky; Carola Schulzke; Prinson P. Samuel; Inorganic Chemistry 49 (2010) 3461–3464; doi:10.1021/ic100031d

data_4315214
_publ_section_title
;
 An Efficient Route for the Synthesis of a Tin(II) Substituted
 Carbodiimide from a Diazo Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3461
_journal_page_last               3464
_journal_paper_doi               10.1021/ic100031d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C37 H50 Fe N4 O4 Si Sn'
_chemical_formula_weight         817.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.764(5)
_cell_length_b                   16.231(3)
_cell_length_c                   10.373(2)
_cell_measurement_reflns_used    15052
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.7
_cell_measurement_theta_min      3.0
_cell_volume                     4001.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  IPDSII
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14172
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.9064
_exptl_absorpt_correction_T_min  0.6385
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.739
_refine_diff_density_min         -2.985
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+9.2823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                3288
_reflns_number_total             3837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100031d_si_001_2.cif
_cod_data_source_block           ja65
_cod_original_cell_volume        4001.3(14)
_cod_database_code               4315214