A crystalline cyclic (alkyl)(amino)carbene with a 1,1‘-ferrocenylene backbone
Volk, Julia; Heinz, Myron; Leibold, Michael; Bruhn, Clemens; Bens, Tobias; Sarkar, Biprajit; Holthausen, Max C.; Siemeling, Ulrich; Chemical Communications  (2022) –; doi:10.1039/D2CC03871D

data_7130566
_publ_section_title
;
 A crystalline cyclic (alkyl)(amino)carbene with a
 1,1&#x2018;-ferrocenylene backbone
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03871D
_journal_year                    2022
_chemical_formula_moiety         'C42 H33 Fe N2 P'
_chemical_formula_sum            'C42 H33 Fe N2 P'
_chemical_formula_weight         652.52
_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             2022-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-01 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                85.398(10)
_cell_angle_beta                 71.395(9)
_cell_angle_gamma                70.741(7)
_cell_formula_units_Z            2
_cell_length_a                   10.1852(8)
_cell_length_b                   12.9446(11)
_cell_length_c                   13.390(2)
_cell_measurement_reflns_used    15723
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      1.61
_cell_volume                     1578.9(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
 207 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  0.0319
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11950
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.269
_diffrn_reflns_theta_min         1.605
_diffrn_source                   'Genix Mo HF'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9117
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0474P)^2^+0.8380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5133
_reflns_number_total             6340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03871d2.cif
_cod_data_source_block           i3327
_cod_database_code               7130566
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42)
;
_shelx_res_checksum              81450
_shelx_hkl_checksum              77515
_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 98.3
_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 52.7
_stoe_evaluation_lana_max_2theta_desired 52.7
_stoe_evaluation_lana_mean_redundancy 1.9
_stoe_evaluation_lana_number_refls_after_or 11951
_stoe_evaluation_lana_number_refls_outliers 1219
_stoe_evaluation_lana_number_refls_total 13170
_stoe_evaluation_lana_number_refls_unique 6341
_stoe_evaluation_lana_number_refls_written 11951
_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 -1
_stoe_evaluation_lana_table
;
2Theta           5.6   11.2   16.8   22.4   28.0   33.6   39.2   44.8   50.4
<Resolution>    6.49   3.51   2.39   1.81   1.46   1.22   1.06   0.93   0.84
N(total)          56    239    502    874   1329   1840   2398   2950   2982
<Redundancy>     2.0    2.0    2.0    1.9    2.0    1.9    1.9    1.9    1.8
Complet. [%%]    96.2   98.2   98.7   99.5  100.0  100.0   99.9   99.8   94.1
<I/sigma>      569.5  320.6  142.3  116.6   67.9   41.7   26.1   15.4    7.8
R(int)         0.039  0.022  0.019  0.019  0.023  0.029  0.037  0.050  0.084
;
_stoe_measurement_identifier     i3327
_stoe_measurement_max_exposure_per_frame '180.0 s'
_stoe_measurement_mean_exposure_per_frame '180.0 s'
_stoe_measurement_min_exposure_per_frame '180.0 s'
_stoe_measurement_total_exposure_time '10.3 h'
_stoe_measurement_total_frame_number 207
_stoe_measurement_total_run_number 2
_stoe_measurement_tube_power     '50.0 W'