Synthesis and X-ray Crystal Structure of [(THF)Zn(O2(OH)SiR)]4 (R = (2,6-i-Pr2C6H3)N(SiMe3)): Enroute to Larger Aggregates
Ganapathi Anantharaman; Herbert W. Roesky; Hans-Georg Schmidt; Mathias Noltemeyer; Jiri Pinkas; Inorganic Chemistry 42 (2003) 970–973; doi:10.1021/ic020514u

data_4313097
_publ_section_title
;
 Synthesis and X-ray Crystal Structure of [(THF)Zn(O2(OH)SiR)]4 (R =
 (2,6-i-Pr2C6H3)N(SiMe3)): Enroute to Larger Aggregates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              970
_journal_page_last               973
_journal_paper_doi               10.1021/ic020514u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C83 H148 N4 O16 Si8 Zn4'
_chemical_formula_weight         1944.25
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.45(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.117(3)
_cell_length_b                   16.692(5)
_cell_length_c                   17.399(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4970(2)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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  0.2388
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6978
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         3.51
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.6653
_exptl_absorpt_correction_T_min  0.5558
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     1498
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+17.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                5623
_reflns_number_total             6928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020514u.cif
_cod_data_source_block           r1008
_cod_database_code               4313097