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_4306400
_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            'C70 H68 Cl4 Cr N5 O6 P2'
_chemical_formula_weight         1331.03
_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                68.179(10)
_cell_angle_beta                 79.346(12)
_cell_angle_gamma                88.643(11)
_cell_formula_units_Z            2
_cell_length_a                   11.961(2)
_cell_length_b                   15.876(3)
_cell_length_c                   18.842(4)
_cell_measurement_reflns_used    1005
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      61.30
_cell_measurement_theta_min      3.00
_cell_volume                     3260.4(11)
_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 0.918
_diffrn_measured_fraction_theta_max 0.918
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25681
_diffrn_reflns_theta_full        61.32
_diffrn_reflns_theta_max         61.32
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    3.867
_exptl_absorpt_correction_T_max  0.9267
_exptl_absorpt_correction_T_min  0.2810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         9249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0504
_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^)+(0.1787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.2110
_reflns_number_gt                7555
_reflns_number_total             9249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801231p_si_002_4.cif
_cod_data_source_block           data0m
_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_cell_volume        3260.5(11)
_cod_database_code               4306400