Influence of Cyclodextrins on Catalytic Olefin Epoxidation with Metal‒Carbonyl Compounds. Crystal Structure of the TRIMEB Complex with CpFe(CO)2Cl
Balula, Salete S.; Coelho, Ana C.; Braga, Susana S.; Hazell, Alan; Valente, Anabela A.; Pillinger, Martyn; Seixas, João D.; Romão, Carlos C.; Gonçalves, Isabel S.; Organometallics 26 (2007) 6857–; doi:10.1021/om701025z

data_4074096
_publ_section_title
;
 Influence of Cyclodextrins on Catalytic Olefin Epoxidation with
 Metal--Carbonyl Compounds. Crystal Structure of the TRIMEB Complex with
 CpFe(CO)2Cl
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6857
_journal_paper_doi               10.1021/om701025z
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C63 H112 O35, C7 H5 Cl1 Fe1 O2'
_chemical_formula_sum            'C70 H117 Cl Fe O37'
_chemical_formula_weight         1642.01
_chemical_name_common            CpFeCl(CO)2TRIMEB
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.189(3)
_cell_length_b                   25.149(6)
_cell_length_c                   28.964(7)
_cell_measurement_reflns_used    4936
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      1.4
_cell_volume                     8150(4)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'Apex2 (Bruker-Nonius, 2003  )'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
;                                    
      ORTEP-III (Burnett & Johnson,   1996), KRYSTAL                      
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                    
     SIR97 (Altomare et al., 1997 ) , KRYSTAL                             
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;                                    
Bruker-Nonius X8Apex-II CCD          
diffractometer                       
;
_diffrn_measurement_method
;                                    
Thin-slice \w and \f scans           
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.170
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            98473
_diffrn_reflns_reduction_process 98473
_diffrn_reflns_theta_full        26.27
_diffrn_reflns_theta_max         26.3
_diffrn_reflns_theta_min         1.4
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.3063
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3504.0
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.2(1)
_refine_diff_density_min         -1.1(1)
_refine_ls_abs_structure_details
;                                    
Rogers factor refimed for 2612 Friedel pairs where both 
I(hkl) and I(-h,k,l) are greater than 3 sigma(I)
;
_refine_ls_abs_structure_Rogers  1.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.404
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.080
_refine_ls_shift/su_max          0.00020
_refine_ls_shift/su_mean         0.00004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;                                    
w= 1/{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^^- |F|}^2^                           
 where A = 0.0500 and B = 5.00
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.090
_reflns_number_gt                6527
_reflns_number_total             16705
_reflns_threshold_expression     'I> 3.\s(I)      '
_cod_data_source_file            om701025z-file003.cif
_cod_data_source_block           TRIMEB
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8150(3)
_cod_original_formula_sum        'C70 H117 Cl1 Fe1 O37'
_cod_database_code               4074096