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_4128577
_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         'C48 H48 Fe O6, 2(Cl4 Fe)'
_chemical_formula_sum            'C48 H48 Cl8 Fe3 O6'
_chemical_formula_weight         1172.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                68.513(3)
_cell_angle_beta                 67.287(3)
_cell_angle_gamma                70.345(3)
_cell_formula_units_Z            1
_cell_length_a                   11.2263(16)
_cell_length_b                   11.4866(16)
_cell_length_c                   12.2107(18)
_cell_measurement_reflns_used    2670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.720
_cell_measurement_theta_min      2.315
_cell_volume                     1316.2(3)
_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      99.95
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.981
_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_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6000
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.745907
_exptl_absorpt_correction_T_min  0.634768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 23873 reflections, Rint = 0.0644
 (8884 with I > 3sig(I), Rint = 0.0452)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.099
_refine_diff_density_max         2.566
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1437P)^2^+2.2330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4053
_reflns_number_total             6000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02613_si_004.cif
_cod_data_source_block           cx1363
_cod_database_code               4128577
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.752
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.526(3)
 0.474(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              29349
_shelx_hkl_checksum              32561
_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 cx1363
_olex2_submission_special_instructions 'No special instructions were received'