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_7714022
_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'
_chemical_formula_sum            'C62 H82 B2 Fe N6'
_chemical_formula_weight         988.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-12
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9740(4)
_cell_length_b                   29.2515(17)
_cell_length_c                   21.3053(9)
_cell_measurement_reflns_used    7348
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.91
_cell_measurement_theta_min      3.02
_cell_volume                     5592.7(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_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(2)
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
 862 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           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10412
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.459
_diffrn_reflns_theta_min         3.021
_diffrn_source                   Cu-Genix
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_target            Cu
_diffrn_source_type              'Genix Cu 3D HF'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.8355
_exptl_absorpt_correction_T_min  0.2403
_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    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.362(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0963P)^2^+1.7532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                2447
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02684a2.cif
_cod_data_source_block           sv1129
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7714022
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.737
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.638(15)
 0.362(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11),
 C12(H12), C22(H22), C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              46742
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '7.0 cm'
_stoe_detector_size_y            '8.4 cm'
_stoe_evaluation_integration_a   4.0
_stoe_evaluation_integration_b   4.0
_stoe_evaluation_integration_ems 0.040
_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 64.0
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 141.1
_stoe_evaluation_lana_max_2theta_desired 141.1
_stoe_evaluation_lana_mean_redundancy 3.0
_stoe_evaluation_lana_number_refls_after_or 10412
_stoe_evaluation_lana_number_refls_outliers 2023
_stoe_evaluation_lana_number_refls_total 12435
_stoe_evaluation_lana_number_refls_unique 3424
_stoe_evaluation_lana_number_refls_written 10412
_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 mm2
_stoe_evaluation_lana_table
;
2Theta          12.8   28.0   43.2   58.4   73.6   88.8  104.0  119.2  134.4
<Resolution>    5.57   3.08   2.07   1.55   1.29   1.09   0.97   0.90   0.84
N(total)          53    226    662   1288   2748   2797   1995   1977    689
<Redundancy>     1.6    1.7    2.0    2.8    4.5    3.9    2.9    2.8    1.8
Complet. [%%]    94.1   87.7   86.3   71.3   68.8   65.7   60.9   60.2   45.8
<I/sigma>      212.1   58.9   26.6   13.1    5.8    3.6    2.4    1.7    1.8
R(int)         0.016  0.023  0.037  0.041  0.088  0.131  0.178  0.242  0.238
;
_stoe_measurement_identifier     sv1129
_stoe_measurement_max_exposure_per_frame '70.0 s'
_stoe_measurement_mean_exposure_per_frame '70.0 s'
_stoe_measurement_min_exposure_per_frame '70.0 s'
_stoe_measurement_total_exposure_time '16.8 h'
_stoe_measurement_total_frame_number 862
_stoe_measurement_total_run_number 17
_stoe_measurement_tube_power     '30.0 W'