Catalyst Behavior in Metal-Catalyzed Carbonyl-Olefin Metathesis.
Hanson, Carly S.; Psaltakis, Mary C.; Cortes, Janiel J.; Devery, 3rd, James J; Journal of the American Chemical Society 141 (2019) 11870–11880; doi:10.1021/jacs.9b02613

data_4128579
_publ_section_title
;
 Catalyst Behavior in Metal-Catalyzed Carbonyl-Olefin Metathesis.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11870
_journal_page_last               11880
_journal_paper_doi               10.1021/jacs.9b02613
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C18 H36 Fe O6, 2(Cl4 Fe)'
_chemical_formula_sum            'C18 H36 Cl8 Fe3 O6'
_chemical_formula_weight         799.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1083(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1760(3)
_cell_length_b                   18.7713(7)
_cell_length_c                   10.2557(4)
_cell_measurement_reflns_used    7136
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.576
_cell_measurement_theta_min      2.471
_cell_volume                     1766.17(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.630
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0681 before and 0.0613 after correction. The Ratio of minimum to maximum transmission is 0.8993. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       tabular
_exptl_crystal_F_000             812
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.4019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4024
_reflns_number_total             4978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02613_si_003.cif
_cod_data_source_block           cx1362
_cod_database_code               4128579
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.701
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl2A)=Sof(Cl3A)=Sof(Cl4A)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl3)=Sof(Cl4)=FVAR(1)
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              63309
_shelx_hkl_checksum              92003
_olex2_date_sample_data_collection 2018-07-26
_olex2_date_sample_submission    2018-07-26
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone'
_olex2_submission_original_sample_id cx1362
_olex2_submission_special_instructions 'No special instructions were received'