Reactivity of hydride bridges in a high-spin [Fe3(μ-H)3]3+ cluster: reversible H2/CO exchange and Fe‒H/B‒F bond metathesis
Anderton, Kevin J.; Knight, Brian J.; Rheingold, Arnold L.; Abboud, Khalil A.; García-Serres, Ricardo; Murray, Leslie J.; Chem. Sci.  (2017) –; doi:10.1039/C6SC05583D

data_1545737
_publ_section_title
;
 Reactivity of hydride bridges in a high-spin [Fe3(\m-H)3]3+ cluster:
 reversible H2/CO exchange and Fe--H/B--F bond metathesis
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C6SC05583D
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H63 F3 Fe3 N6'
_chemical_formula_sum            'C45 H63 F3 Fe3 N6'
_chemical_formula_weight         912.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-07-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_audit_update_record
;
2016-12-21 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.429(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7273(14)
_cell_length_b                   11.4948(8)
_cell_length_c                   21.957(2)
_cell_measurement_reflns_used    4698
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.214
_cell_measurement_theta_min      2.468
_cell_volume                     4835.7(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16564
_diffrn_reflns_point_group_measured_fraction_full 0.738
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         2.583
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0582 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8271.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1848 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7136
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.446
_reflns_Friedel_fraction_full    0.479
_reflns_Friedel_fraction_max     0.445
_reflns_number_gt                6403
_reflns_number_total             7136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05583d2.cif
_cod_data_source_block           ccnow_a_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1545737
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.773
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C31(H31A,H31B), C29(H29A,H29B), C30(H30A,H30B), C44(H44A,
 H44B), C45(H45A,H45B), C25(H25A,H25B), C42(H42A,H42B), C23(H23A,H23B),
 C38(H38A,H38B), C40(H40A,H40B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C13(H13)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C28(H28A,H28B,H28C), C15(H15A,H15B,H15C),
 C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C43(H43A,H43B,H43C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              78692
_shelx_fab_checksum              26770
_olex2_submission_special_instructions 'No special instructions were received'