X-ray Diffraction and 2D Gradient-Assisted1H−119Sn HMQC NMR Studies of Structures Obtained from Nucleophilic Substitutions on Dimethyltin(IV) Salicylaldoximates
Willem, Rudolph; Bouhdid, Abdeslam; Meddour, Abdelkrim; Camacho-Camacho, Carlos; Mercier, Frédéric; Gielen, Marcel; Biesemans, Monique; Ribot, François; Sanchez, Clément; Tiekink, Edward R. T.; Organometallics 16 (1997) 4377–; doi:10.1021/om970378e

data_4078376
_publ_section_title
;
 X-ray Diffraction and 2D Gradient-Assisted1H&#x2212;119Sn HMQC NMR
 Studies of Structures Obtained from Nucleophilic Substitutions on
 Dimethyltin(IV) Salicylaldoximates
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4377
_journal_paper_doi               10.1021/om970378e
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C29 H36 Br N2 O6 Sn3'
_chemical_formula_weight         944.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Jan 10 15:36:43 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                105.09(7)
_cell_angle_beta                 113.43(6)
_cell_angle_gamma                87.26(7)
_cell_formula_units_Z            2
_cell_length_a                   11.765(9)
_cell_length_b                   15.76(1)
_cell_length_c                   10.205(8)
_cell_measurement_reflns_used    5
_cell_measurement_temperature    293
_cell_measurement_theta_max      49.8
_cell_measurement_theta_min      49.4
_cell_volume                     1673(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      293
_diffrn_measurement_device       AFC6R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.01446
_diffrn_orient_matrix_UB_12      -0.05426
_diffrn_orient_matrix_UB_13      0.03644
_diffrn_orient_matrix_UB_21      0.07786
_diffrn_orient_matrix_UB_22      -0.00769
_diffrn_orient_matrix_UB_23      -0.01808
_diffrn_orient_matrix_UB_31      0.04841
_diffrn_orient_matrix_UB_32      0.03650
_diffrn_orient_matrix_UB_33      0.10296
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8098
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -4.05
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.460
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             914.00
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.631
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0377
_refine_ls_shift/esd_max         0.0048
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0335
_reflns_number_observed          4611
_reflns_number_total             7724
_reflns_observed_criterion       3.00
_cod_data_source_file            om970378e.cif
_cod_data_source_block           5b
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C29 H36 Br N2 O6 Sn3 '
_cod_database_code               4078376