Mechanistic Insight into the Initiation Step of the Coupling Reaction of Oxetane or Epoxides and CO2 Catalyzed by (salen)CrX Complexes
Donald J. Darensbourg; Adriana I. Moncada; Inorganic Chemistry 47 (2008) 10000–10008; doi:10.1021/ic801231p

data_4306398
_publ_section_title
;
Mechanistic Insight into the Initiation Step of the Coupling Reaction of
Oxetane or Epoxides and CO2 Catalyzed by (salen)CrX Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10000
_journal_page_last               10008
_journal_paper_doi               10.1021/ic801231p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C67.5 H67 Cl3 Cr N6 O4 P'
_chemical_formula_weight         1215.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.026(8)
_cell_angle_beta                 82.558(9)
_cell_angle_gamma                79.978(9)
_cell_formula_units_Z            2
_cell_length_a                   12.447(2)
_cell_length_b                   15.076(2)
_cell_length_c                   18.509(3)
_cell_measurement_reflns_used    3561
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      57.72
_cell_measurement_theta_min      2.55
_cell_volume                     3205.3(9)
_computing_cell_refinement
;
 CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003)
;
_computing_data_collection       'FRAMBO (BRUKER-NONIUS, 2003)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_sigmaI/netI    0.1425
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21367
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         4.66
_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_T_max  0.9376
_exptl_absorpt_correction_T_min  0.3154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     565
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1430P)^2^+4.4531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2131
_refine_ls_wR_factor_ref         0.2716
_reflns_number_gt                4397
_reflns_number_total             8449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801231p_si_002_2.cif
_cod_data_source_block           dda
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_formula_sum        'C67.50 H67 Cl3 Cr N6 O4 P'
_cod_database_code               4306398