Ferrocene Tethered Boramidinate Frustrated Lewis Pairs: Stepwise Capture of CO2 and CO
Esarte Palomero, Orhi; Jones, Richard A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00691J

data_7709874
_publ_section_title
;
 Ferrocene Tethered Boramidinate Frustrated Lewis Pairs: Stepwise Capture
 of CO2 and CO
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00691J
_journal_year                    2022
_chemical_formula_moiety         'C46 H28 B2 F20 Fe N4 O3, C H2 Cl2'
_chemical_formula_sum            'C47 H30 B2 Cl2 F20 Fe N4 O3'
_chemical_formula_weight         1227.12
_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             2019-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-30 deposited with the CCDC.	2022-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 88.897(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1533(5)
_cell_length_b                   17.1798(9)
_cell_length_c                   26.935(2)
_cell_measurement_reflns_used    5273
_cell_measurement_temperature    100.0(7)
_cell_measurement_theta_max      75.1730
_cell_measurement_theta_min      3.0280
_cell_volume                     5160.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  30.00   1.00   30.00    --  -39.84  57.00  60.00   93
  2  \w    -64.00  29.00   1.00   30.00    --  -39.84  38.00 -30.00   93
  3  \w   -113.00 -20.00   1.00   30.00    --  -39.84 -38.00 150.00   93
  4  \w   -126.00 -34.00   1.00   30.00    --  -39.84 178.00   0.00   92
  5  \w     87.00 129.00   1.00   30.00    --   39.84 178.00  30.00   42
  6  \w     39.00  74.00   1.00   65.00    --  112.00 -45.00 120.00   35
  7  \w     90.00 178.00   1.00   65.00    --  112.00  30.00   0.00   88
  8  \w     95.00 178.00   1.00   65.00    --  112.00  30.00 -60.00   83
  9  \w     77.00 108.00   1.00   65.00    --  112.00 -94.00 -30.00   31
 10  \w     31.00  61.00   1.00   65.00    --  112.00 -94.00 -30.00   30
 11  \w     38.00 111.00   1.00   65.00    --  112.00-111.00 120.00   73
 12  \w     84.00 173.00   1.00   65.00    --  112.00  30.00  60.00   89
 13  \w    100.00 176.00   1.00   65.00    --  112.00 111.00-120.00   76
 14  \w     29.00 108.00   1.00   65.00    --  112.00 -94.00-150.00   79
 15  \w     93.00 138.00   1.00   65.00    --  112.00  45.00-120.00   45
 16  \w     71.00 113.00   1.00   65.00    --  112.00-111.00  60.00   42
 17  \w     88.00 126.00   1.00   65.00    --  112.00 -45.00 120.00   38
 18  \w    150.00 177.00   1.00   65.00    --  112.00  45.00-120.00   27
 19  \w     29.00 109.00   1.00   65.00    --  112.00 -94.00 150.00   80
 20  \w     53.00 131.00   1.00   65.00    --  112.00 -61.00-120.00   78
 21  \w     37.00 110.00   1.00   65.00    --  112.00 -94.00 -90.00   73
 22  \w     44.00  69.00   1.00   65.00    --  112.00 -45.00 -60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1333157000
_diffrn_orient_matrix_UB_12      -0.0141379000
_diffrn_orient_matrix_UB_13      -0.0110582000
_diffrn_orient_matrix_UB_21      0.0282695000
_diffrn_orient_matrix_UB_22      0.0055931000
_diffrn_orient_matrix_UB_23      -0.0560855000
_diffrn_orient_matrix_UB_31      0.0230476000
_diffrn_orient_matrix_UB_32      -0.0883570000
_diffrn_orient_matrix_UB_33      -0.0017840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35425
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.370
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_recrystallization_method
'Slow vapour diffusion of pentane into a dichloromethane solution'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.853
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         9460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_gt           0.1465
_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^)+(0.1027P)^2^+100.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3512
_refine_ls_wR_factor_ref         0.3626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7135
_reflns_number_total             9460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           opegfcpierscoco2_2_numericalabs_rintfilter
_cod_database_code               7709874
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         FeCl2F20B2N4O3C47H30
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.433
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C25(H25), C3(H3), C28(H28), C29(H29), C24(H24), C27(H27), C23(H23),
 C22(H22), C26(H26)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31094
_shelx_fab_checksum              1931
_olex2_exptl_crystal_mounting_method
'Coated in paratone oil. Mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.118
_oxdiff_exptl_absorpt_empirical_full_min 0.411