Synthesis and Structure of Zwitterionic Silylborates and Silylzincates with Pendant Polydonor Arms
Li, Hui; Hung-Low, Fernando; Krempner, Clemens; Organometallics 31 (2012) 7117–; doi:10.1021/om300652n

data_4079289
_publ_section_title
;
 Synthesis and Structure of Zwitterionic Silylborates and Silylzincates
 with Pendant Polydonor Arms
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7117
_journal_paper_doi               10.1021/om300652n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C90 H220 I12 K6 O36 Si24 Zn6'
_chemical_formula_weight         4702.44
_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                 95.030(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   26.705(4)
_cell_length_b                   19.098(3)
_cell_length_c                   18.507(3)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.58
_cell_volume                     9402(3)
_computing_cell_refinement       'Bruker APEX 2'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker APEX 2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            92585
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    3.063
_exptl_absorpt_correction_T_max  0.545
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4628
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.198
_refine_diff_density_max         3.821
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         17035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+100.8438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1527
_reflns_number_gt                12716
_reflns_number_total             17035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300652n_si_002.cif
_cod_data_source_block           ck
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        9403(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4079289