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_7709876
_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         'C48 H67 B2 Fe N4'
_chemical_formula_sum            'C48 H67 B2 Fe N4'
_chemical_formula_weight         777.52
_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             2018-11-09
_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                103.457(5)
_cell_angle_beta                 91.662(5)
_cell_angle_gamma                90.120(7)
_cell_formula_units_Z            2
_cell_length_a                   6.8547(6)
_cell_length_b                   16.8578(13)
_cell_length_c                   18.2501(9)
_cell_measurement_reflns_used    3281
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      74.6610
_cell_measurement_theta_min      3.2000
_cell_volume                     2050.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.942
_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    -67.00  26.00   1.00   11.00    --  -42.67  57.00 -30.00   93
  2  \w     47.00 133.00   1.00   38.50    --  111.00 -61.00-150.00   86
  3  \w   -111.00 -18.00   1.00   11.00    --  -42.67 -57.00-180.00   93
  4  \w     87.00 114.00   1.00   38.50    --  111.00  77.00 -30.00   27
  5  \w    -25.00  74.00   1.00   11.00    --   42.67 -77.00  60.00   99
  6  \w     93.00 178.00   1.00   38.50    --  111.00  30.00 -60.00   85
  7  \w     40.00  74.00   1.00   38.50    --  111.00-125.00 -90.00   34
  8  \w     39.00 110.00   1.00   38.50    --  111.00-125.00  60.00   71
  9  \w     77.00 117.00   1.00   38.50    --  111.00-125.00 -90.00   40
 10  \w    127.00 178.00   1.00   38.50    --  111.00  77.00 -30.00   51
 11  \w     45.00 138.00   1.00   38.50    --  111.00 -61.00   0.00   93
 12  \w     40.00 117.00   1.00   38.50    --  111.00-125.00-150.00   77
 13  \w    114.00 140.00   1.00   38.50    --  111.00 125.00-150.00   26
 14  \w    150.00 175.00   1.00   38.50    --  111.00 125.00-150.00   25
 15  \w     68.00 175.00   1.00   38.50    --  111.00  15.00  60.00  107
;
_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      -0.1357311000
_diffrn_orient_matrix_UB_12      0.0732323000
_diffrn_orient_matrix_UB_13      0.0023671000
_diffrn_orient_matrix_UB_21      -0.1706085000
_diffrn_orient_matrix_UB_22      -0.0486877000
_diffrn_orient_matrix_UB_23      0.0217479000
_diffrn_orient_matrix_UB_31      0.0550338000
_diffrn_orient_matrix_UB_32      0.0331285000
_diffrn_orient_matrix_UB_33      0.0840352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13182
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.481
_diffrn_reflns_theta_min         2.695
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_recrystallization_method
'Crystallized from toluene solution at room temperature'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8117
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0822
_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^)+(0.1327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6044
_reflns_number_total             8117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           fcada9bbn-fullpt75
_cod_database_code               7709876
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C48H28N8Fe
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.583
_reflns_odcompleteness_completeness 96.20
_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
2. Restrained distances
 C46-C47 \\sim C35-C40
 with sigma of 0.02
 C46-C41 \\sim C35-C32
 with sigma of 0.02
 C46-C45 \\sim C35-C36
 with sigma of 0.02
 C49-C44 \\sim C38-C37
 with sigma of 0.02
 C49-C48 \\sim C38-C39
 with sigma of 0.02
 C50-C42 \\sim C31-C34
 with sigma of 0.02
 C50-C43 \\sim C31-C33
 with sigma of 0.02
 C50-C41 \\sim C31-C32
 with sigma of 0.02
 C50-N4 \\sim C31-N1A
 with sigma of 0.02
 C30-N4 \\sim C30-N1A
 with sigma of 0.02
 C44-C43 \\sim C37-C33
 with sigma of 0.02
 C44-C45 \\sim C37-C36
 with sigma of 0.02
 C48-C42 \\sim C39-C34
 with sigma of 0.02
 C48-C47 \\sim C39-C40
 with sigma of 0.02
 C46-C50 \\sim C35-C31
 with sigma of 0.04
 C46-C44 \\sim C35-C37
 with sigma of 0.04
 C46-C48 \\sim C35-C39
 with sigma of 0.04
 C49-C42 \\sim C38-C34
 with sigma of 0.04
 C49-C47 \\sim C38-C40
 with sigma of 0.04
 C49-C43 \\sim C38-C33
 with sigma of 0.04
 C49-C45 \\sim C38-C36
 with sigma of 0.04
 C50-C30 \\sim C31-C30
 with sigma of 0.04
 C50-C44 \\sim C31-C37
 with sigma of 0.04
 C50-C48 \\sim C31-C39
 with sigma of 0.04
 C44-C48 \\sim C37-C39
 with sigma of 0.04
 C42-C47 \\sim C34-C40
 with sigma of 0.04
 C42-C43 \\sim C34-C33
 with sigma of 0.04
 C42-C41 \\sim C34-C32
 with sigma of 0.04
 C42-N4 \\sim C34-N1A
 with sigma of 0.04
 C47-C41 \\sim C40-C32
 with sigma of 0.04
 C47-C45 \\sim C40-C36
 with sigma of 0.04
 C43-C41 \\sim C33-C32
 with sigma of 0.04
 C43-C45 \\sim C33-C36
 with sigma of 0.04
 C43-N4 \\sim C33-N1A
 with sigma of 0.04
 C41-C45 \\sim C32-C36
 with sigma of 0.04
 C41-N4 \\sim C32-N1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C39)=Sof(H39)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C37)=Sof(H37)=Sof(C31)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(N1A)=1-FVAR(1)
 Sof(C46)=Sof(H46)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(C44)=Sof(H44)=
 Sof(C48)=Sof(H48)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(N4)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C55(H55), C17(H17), C21(H21), C46(H46), C11(H11), C51(H51), C15(H15),
 C13(H13), C44(H44), C48(H48), C35(H35), C39(H39), C37(H37)
5.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C8(H8A,H8B), C23(H23A,H23B), C14(H14A,H14B), C58(H58A,H58B),
 C57(H57A,H57B), C20(H20A,H20B), C56(H56A,H56B), C9(H9A,H9B), C54(H54A,H54B),
 C10(H10A,H10B), C49(H49A,H49B), C53(H53A,H53B), C18(H18A,H18B), C22(H22A,H22B),
  C19(H19A,H19B), C52(H52A,H52B), C12(H12A,H12B), C16(H16A,H16B), C42(H42A,
 H42B), C47(H47A,H47B), C43(H43A,H43B), C41(H41A,H41B), C45(H45A,H45B),
 C32(H32A,H32B), C36(H36A,H36B), C40(H40A,H40B), C38(H38A,H38B), C34(H34A,H34B),
  C33(H33A,H33B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C3(H3), C26(H26), C5(H5), C27(H27), C29(H29), C4(H4), C28(H28)
;
_shelx_res_checksum              17402
_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 2.266
_oxdiff_exptl_absorpt_empirical_full_min 0.626