Di- and Tri-Zinc Catalysts for the Low-Pressure Copolymerization of CO2 and Cyclohexene Oxide
Michael R. Kember; Andrew J. P. White; Charlotte K. Williams; Inorganic Chemistry 48 (2009) 9535–9542; doi:10.1021/ic901109e

data_4303261
_publ_section_title
;
Di- and Tri-Zinc Catalysts for the Low-Pressure Copolymerization of CO2 and
Cyclohexene Oxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9535
_journal_page_last               9542
_journal_paper_doi               10.1021/ic901109e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C36 H54 N4 O10 Zn3, 1.75(C4 H8 O)'
_chemical_formula_sum            'C43 H68 N4 O11.75 Zn3'
_chemical_formula_weight         1025.12
_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                 114.217(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.2406(3)
_cell_length_b                   16.3317(2)
_cell_length_c                   29.4556(2)
_cell_measurement_reflns_used    48529
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.7025
_cell_measurement_theta_min      3.8394
_cell_volume                     10635.0(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173(2)
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            136789
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.76
_diffrn_reflns_theta_min         3.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
 SQUEEZE suggests 589e/cell, which is 147.25e/asu or 73.6e/complex.
 Before SQUEEZE, solvent looked like thf in 6 different sites per asu.
 thf = C4H8O = 40e, 1.75thf = 70e. This is close to the 73.6e/complex
 suggested by SQUEEZE so this was considered to be the solvent present.

 asu thus 3.5thf low = C14 H28 O3.5, so UNIT C56 H112 O14 low,
 i.e. C288 H432 N32 O80 Zn24
;
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         33259
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2331
_reflns_number_gt                18559
_reflns_number_total             33259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901109e_si_002_2.cif
_cod_data_source_block           '[L2Zn3(OAc)4]'
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303261