Copolymerization of Cyclohexene Oxide and CO2 with a Chromium Diamine-bis(phenolate) Catalyst
Rebecca K. Dean; Louise N. Dawe; Christopher M. Kozak; Inorganic Chemistry 51 (2012) 9095–9103; doi:10.1021/ic301402z

data_4330123
_publ_contact_author_address
;
Department of chemistry
Memorial University of Newfoundland
St. Johns, NL, A1B 3X7, Canada
;
_publ_contact_author_email       ckozak@mun.ca
_publ_contact_author_fax         1-709-864-3702
_publ_contact_author_name        'Christopher Kozak'
_publ_contact_author_phone       1-709-864-8082
_publ_section_title
;
 Copolymerization of Cyclohexene Oxide and CO2 with a Chromium
 Diamine-bis(phenolate) Catalyst
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9095
_journal_page_last               9103
_journal_paper_doi               10.1021/ic301402z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C72 H100 Cl2 Cr2 N4 O4, 2.5(C6 H6)'
_chemical_formula_sum            'C87 H115 Cl2 Cr2 N4 O4'
_chemical_formula_weight         1455.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 109.020(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.3979(12)
_cell_length_b                   13.4522(10)
_cell_length_c                   21.3183(17)
_cell_measurement_reflns_used    35626
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4174.7(6)
_computing_cell_refinement
'PROCESS-AUTO CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection
'PROCESS-AUTO CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53858
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1558
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 54 electrons per 
unit cell in two voids (total volume 478 ^A^3); that is, 27 electrons per
formula unit. This electron density is attributed to 0.5 occupancy 
disordered solvent lattice benzene molecule (21 eletrons) for which a 
good point atom model could not be achieved. The application of 
Squeeze gave a good improvement in the data statistics and allowed for a 
full anisotropic refinement of the  structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         8649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0701P)^2^+4.0103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                6766
_reflns_number_total             8649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301402z_si_002.cif
_cod_data_source_block           Cmpd1
_cod_database_code               4330123