A complete series of N-heterocyclic tetrylenes (Si – Pb) with a 1,1’-ferrocenediyl backbone enabled by 1,3,2-diazaborolyl N-substituents
Guthardt, Robin; Jacob, Hannes Lukas; Bruhn, Clemens; Siemeling, Ulrich; Dalton Transactions  (2023) –; doi:10.1039/D3DT02684A

data_7714026
_publ_section_title
;
 A complete series of N-heterocyclic tetrylenes (Si -- Pb) with a
 1,1&#x2019;-ferrocenediyl backbone enabled by 1,3,2-diazaborolyl
 N-substituents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02684A
_journal_year                    2023
_chemical_formula_moiety         'C62 H82 B2 Fe N6 O Si'
_chemical_formula_sum            'C62 H82 B2 Fe N6 O Si'
_chemical_formula_weight         1032.89
_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             2023-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-16 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.103(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2033(8)
_cell_length_b                   23.7917(17)
_cell_length_c                   19.6371(12)
_cell_measurement_reflns_used    22476
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      1.35
_cell_volume                     5697.5(7)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
 140 frames, detector distance = 125 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2, 0.6 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25310
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         1.345
_diffrn_source                   'Genix Mo HF'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.8677
_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, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0850
_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^)+(0.1744P)^2^+1.0753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7801
_reflns_number_total             11500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02684a2.cif
_cod_data_source_block           i3328
_cod_database_code               7714026
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: Si1(0.5) H1(0.5) Si1A(0.5) H1A(0.5) O1(0.5) H1B(0.5) O1A(0.5)
 H1AA(0.5)
3.a Ternary CH refined with riding coordinates:
 Si1(H1), Si1A(H1A), C19(H19), C22(H22), C31(H31), C34(H34), C45(H45),
 C48(H48), C57(H57), C60(H60)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28), C29(H29), C37(H37),
  C38(H38), C41(H41), C42(H42), C43(H43), C53(H53), C54(H54), C55(H55)
3.c Tetrahedral OH refined with riding coordinates:
 O1(H1B)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C)
3.e Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA)
;
_shelx_res_checksum              77702
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '125.0 mm'
_stoe_detector_pixelsize_x       '0.150 mm'
_stoe_detector_pixelsize_y       '0.150 mm'
_stoe_detector_size_x            '34.0 cm'
_stoe_detector_size_y            '34.0 cm'
_stoe_evaluation_integration_a   12.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max -
_stoe_evaluation_lana_bos_l_odd_max -
_stoe_evaluation_lana_completeness 98.7
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 52.7
_stoe_evaluation_lana_max_2theta_desired 52.7
_stoe_evaluation_lana_mean_redundancy 2.2
_stoe_evaluation_lana_number_refls_after_or 25314
_stoe_evaluation_lana_number_refls_outliers 6577
_stoe_evaluation_lana_number_refls_total 31891
_stoe_evaluation_lana_number_refls_unique 11502
_stoe_evaluation_lana_number_refls_written 25314
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           4.5   10.3   16.1   21.9   27.7   33.5   39.3   45.1   50.9
<Resolution>    7.10   3.78   2.49   1.85   1.47   1.23   1.05   0.92   0.84
N(total)          98    469   1167   2112   3237   4558   6014   7585   6651
<Redundancy>     2.2    2.2    2.2    2.2    2.2    2.2    2.2    2.2    2.2
Complet. [%%]   100.0   98.8   99.0   99.9  100.0  100.0  100.0  100.0   94.8
<I/sigma>      557.6  289.3  106.0   66.7   33.9   17.8   10.1    4.6    2.4
R(int)         0.028  0.051  0.055  0.060  0.058  0.064  0.081  0.113  0.173
;
_stoe_measurement_identifier     i3328
_stoe_measurement_max_exposure_per_frame '300.0 s'
_stoe_measurement_mean_exposure_per_frame '300.0 s'
_stoe_measurement_min_exposure_per_frame '300.0 s'
_stoe_measurement_total_exposure_time '11.7 h'
_stoe_measurement_total_frame_number 140
_stoe_measurement_total_run_number 1
_stoe_measurement_tube_power     '50.0 W'