Experimental and Computational Investigation of the Mechanism of Carbon Dioxide/Cyclohexene Oxide Copolymerization Using a Dizinc Catalyst
Buchard, Antoine; Jutz, Fabian; Kember, Michael R.; White, Andrew J. P.; Rzepa, Henry S.; Williams, Charlotte K.; Macromolecules 45 (2012) 6781–; doi:10.1021/ma300803b

data_1508548
_publ_section_title
;
 Experimental and Computational Investigation of the Mechanism of Carbon
 Dioxide/Cyclohexene Oxide Copolymerization Using a Dizinc Catalyst
;
_journal_issue                   17
_journal_name_full               Macromolecules
_journal_page_first              6781
_journal_paper_doi               10.1021/ma300803b
_journal_volume                  45
_journal_year                    2012
_chemical_formula_moiety         'C44 H74 N4 O7 Zn2, 3.25(C4 H8 O)'
_chemical_formula_sum            'C57 H100 N4 O10.25 Zn2'
_chemical_formula_weight         1136.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_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            8
_cell_length_a                   32.15167(18)
_cell_length_b                   32.15167(18)
_cell_length_c                   12.28484(10)
_cell_measurement_reflns_used    39216
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.3825
_cell_measurement_theta_min      1.9416
_cell_volume                     12699.21(14)
_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
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            99414
_diffrn_reflns_theta_full        72.53
_diffrn_reflns_theta_max         72.53
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 SQUEEZE suggested 1025 e/cell = 256.3 e/asu = 128.1 e/Zn2
 The solvents used were hexane and thf.
 Before SQUEEZE the solvent looked most like thf (C4H8O) = 40e.
 3.25thf = 130e so this was used as the solvent present.
 
 The N-H protons were not located and so were added in idealised
 positions. The H2O protons were not included, so the asu is 4H low
 
 Thus asu is low by 6.5(C4H8O) + 4H = C26 H56 O6.5, and the
 UNIT low by C104 H224 O26,
 i.e. C352 H576 N32 O56 Zn16
;
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 11522 Friedel pairs'
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         24669
_refine_ls_number_restraints     928
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+7.0655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                21479
_reflns_number_total             24669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma300803b_si_004.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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        12699.20(16)
_cod_original_sg_symbol_H-M      P-4
_cod_database_code               1508548