Influence of structural and electronic properties of organomolybdenum(ii) complexes of the type [CpMo(CO)3R] and [CpMo(O2)(O)R] (R = Cl, CH3, CF3) on the catalytic olefin epoxidation
Hauser, Simone A.; Reich, Robert M.; Mink, János; Pöthig, Alexander; Cokoja, Mirza; Kühn, Fritz E.; Catal. Sci. Technol. 5 (2015) 2282–; doi:10.1039/C4CY01604A

data_1518546
_publ_section_title
;
 Influence of structural and electronic properties of organomolybdenum(ii)
 complexes of the type [CpMo(CO)3R] and [CpMo(O2)(O)R] (R = Cl, CH3, CF3)
 on the catalytic olefin epoxidation
;
_journal_issue                   4
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              2282
_journal_paper_doi               10.1039/C4CY01604A
_journal_volume                  5
_journal_year                    2015
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C9 H5 F3 Mo O3'
_chemical_formula_sum            'C9 H5 F3 Mo O3'
_chemical_formula_weight         314.07
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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_update_record
;
2014-10-23 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                107.752(1)
_cell_angle_beta                 97.132(1)
_cell_angle_gamma                107.192(1)
_cell_formula_units_Z            1
_cell_length_a                   6.4530(2)
_cell_length_b                   6.5440(2)
_cell_length_c                   6.7851(2)
_cell_measurement_reflns_used    8174
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3472
_cell_measurement_theta_min      3.2434
_cell_volume                     253.356(14)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            910
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS, Bruker, 2012'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             152
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         910
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0147
_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^)+(0.0147P)^2^+0.3456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0381
_reflns_number_gt                905
_reflns_number_total             910
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cy01604a2.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 1518546--1518547.cif.
;
_cod_database_code               1518546