Reactivity of an N-heterocyclic silylene with a 1,1'-ferrocenediyl backbone towards carbonyl compounds, including carbon suboxide.
Weyer, Nadine; Heinz, Myron; Bruhn, Clemens; Holthausen, Max C.; Siemeling, Ulrich; Chemical communications (Cambridge, England) 57 (2021) 9378–9381; doi:10.1039/d1cc03947d

data_7128845
_publ_section_title
;
 Reactivity of an N-heterocyclic silylene with a 1,1'-ferrocenediyl
 backbone towards carbonyl compounds, including carbon suboxide.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9378
_journal_page_last               9381
_journal_paper_doi               10.1039/d1cc03947d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C73 H84 Fe2 N4 O3 Si2, 1.5(C6 H6)'
_chemical_formula_sum            'C82 H93 Fe2 N4 O3 Si2'
_chemical_formula_weight         1350.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2021-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.132(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.180(3)
_cell_length_b                   22.128(2)
_cell_length_c                   20.694(4)
_cell_measurement_reflns_used    28554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.47
_cell_measurement_theta_min      2.93
_cell_volume                     6911(2)
_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(2)
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details
;
 767 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24200
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.902
_diffrn_reflns_theta_min         2.933
_diffrn_source                   Cu-Genix
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.108
_exptl_absorpt_correction_T_max  0.6211
_exptl_absorpt_correction_T_min  0.1813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       plate
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.995
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         12476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+20.1629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9917
_reflns_number_total             12476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03947d2.cif
_cod_data_source_block           sv0994
_cod_depositor_comments
'Adding full bibliography for 7128840--7128846.cif.'
_cod_original_cell_volume        6911.5(19)
_cod_database_code               7128845
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.344
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H73A,H73B,H73C} of C73, {H72A,H72B,H72C} of C72, {H61A,
  H61B,H61C} of C61, {H69A,H69B,H69C} of C69, {H57A,H57B,H57C} of C57, {H60A,
  H60B,H60C} of C60, {H58A,H58B,H58C} of C58, {H24A,H24B,H24C} of C24, {H23A,
  H23B,H23C} of C23, {H26A,H26B,H26C} of C26, {H27A,H27B,H27C} of C27, {H36A,
  H36B,H36C} of C36, {H35A,H35B,H35C} of C35, {H38A,H38B,H38C} of C38, {H39A,
  H39B,H39C} of C39
 At 1.5 times of:
  {H70A,H70B,H70C} of C70
2.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C34(H34), C37(H37), C56(H56), C59(H59), C68(H68), C71(H71)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C41(H41), C42(H42),
  C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52),
 C53(H53), C54(H54), C64(H64), C65(H65), C66(H66), C74(H74), C75(H75), C76(H76),
  C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C),
 C61(H61A,H61B,H61C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,
 H72C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              12213
_olex2_submission_special_instructions 'No special instructions were received'