Planar-chiral 1,1’-diaminoferrocenes
Guthardt, Robin; Blanckenberg, Johannes; Bruhn, Clemens; Siemeling, Ulrich; Chemical Communications  (2021) –; doi:10.1039/D1CC05287J

data_7129239
_publ_section_title
;
 Planar-chiral 1,1&#x2019;-diaminoferrocenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05287J
_journal_year                    2021
_chemical_formula_moiety         'C28 H35 Fe N2 P Pb Si2'
_chemical_formula_sum            'C28 H35 Fe N2 P Pb Si2'
_chemical_formula_weight         749.77
_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             2020-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                106.545(8)
_cell_angle_beta                 93.996(7)
_cell_angle_gamma                108.683(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3749(9)
_cell_length_b                   11.2394(14)
_cell_length_c                   15.5017(12)
_cell_measurement_reflns_used    27724
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.61
_cell_measurement_theta_min      3.02
_cell_volume                     1615.5(3)
_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_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
 1565 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_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13110
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.923
_diffrn_reflns_theta_min         4.391
_exptl_absorpt_coefficient_mu    14.919
_exptl_absorpt_correction_T_max  0.5610
_exptl_absorpt_correction_T_min  0.0774
_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    1.541
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+2.4495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             5933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05287j2.cif
_cod_data_source_block           sv0888
_cod_database_code               7129239
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.689
_shelx_estimated_absorpt_t_min   0.170
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              70351
_shelx_hkl_checksum              44288
_shelx_fab_checksum              72291
_olex2_submission_special_instructions 'No special instructions were received'