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

data_7129237
_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         'C32 H50 Cl Fe N2 Rh Si'
_chemical_formula_sum            'C32 H50 Cl Fe N2 Rh Si'
_chemical_formula_weight         685.04
_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             2020-11-09
_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                96.230(4)
_cell_angle_beta                 98.922(4)
_cell_angle_gamma                94.876(4)
_cell_formula_units_Z            4
_cell_length_a                   10.0905(5)
_cell_length_b                   18.0609(9)
_cell_length_c                   18.3689(9)
_cell_measurement_reflns_used    23934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.50
_cell_volume                     3269.9(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                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
 204 frames, detector distance = 120 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25921
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.847
_diffrn_reflns_theta_min         2.054
_diffrn_source                   'Genix Mo HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.5078
_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    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13789
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0773P)^2^+4.1308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9432
_reflns_number_total             13789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05287j2.cif
_cod_data_source_block           i3025
_cod_database_code               7129237
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C59, C60, C63, C64, C31, C32, C28, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
 C13, C12, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
3.a Ternary CH refined with riding coordinates:
 C25(H25), C26(H26), C29(H29), C30(H30), C38(H38), C57(H57), C58(H58),
 C61(H61), C62(H62)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C17(H17A,H17B), C27(H27A,H27B), C28(H28A,H28B), C31(H31A,
 H31B), C32(H32A,H32B), C44(H44A,H44B), C49(H49A,H49B), C59(H59A,H59B),
 C60(H60A,H60B), C63(H63A,H63B), C64(H64A,H64B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C36(H36),
 C37(H37), C40(H40), C41(H41), C42(H42), C43(H43)
3.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              4626
_shelx_hkl_checksum              44029
_shelx_fab_checksum              14507
_olex2_submission_special_instructions 'No special instructions were received'