Preparation, X-ray Structures, and NMR Spectra of Elongated Dihydrogen Complexes with Four- and Five-Coordinate Tin Centers
Eguillor, Beatriz; Esteruelas, Miguel A.; Oliván, Montserrat; Organometallics 25 (2006) 4691–; doi:10.1021/om060395g

data_4075603
_publ_section_title
;
 Preparation, X-ray Structures, and NMR Spectra of Elongated Dihydrogen
 Complexes with Four- and Five-Coordinate Tin Centers
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4691
_journal_paper_doi               10.1021/om060395g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C38 H59 Cl O4 Os P2 Sn'
_chemical_formula_weight         986.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   11.6836(5)
_cell_length_b                   15.6616(7)
_cell_length_c                   21.8655(10)
_cell_measurement_reflns_used    8850
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     4001.0(3)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50644
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.980
_exptl_absorpt_correction_T_max  0.654
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         10027
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.190
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0526
_reflns_number_gt                9126
_reflns_number_total             10027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060395gsi20060704_033459.cif
_cod_data_source_block           mae156as
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4075603