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

data_7129244
_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         'C60 H99 Fe3 Li9 N6 O3 Si6'
_chemical_formula_sum            'C60 H99 Fe3 Li9 N6 O3 Si6'
_chemical_formula_weight         1351.00
_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   mixed
_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                107.662(6)
_cell_angle_beta                 94.249(6)
_cell_angle_gamma                96.501(6)
_cell_formula_units_Z            2
_cell_length_a                   12.5721(8)
_cell_length_b                   16.4696(14)
_cell_length_c                   20.0781(16)
_cell_measurement_reflns_used    58006
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.90
_cell_measurement_theta_min      2.32
_cell_volume                     3910.0(5)
_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                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details
;
 1593 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           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29514
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.010
_diffrn_reflns_theta_min         3.562
_diffrn_source                   Cu-Genix
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.590
_exptl_absorpt_correction_T_max  0.4053
_exptl_absorpt_correction_T_min  0.1202
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       plate
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         14270
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0861P)^2^+9.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12715
_reflns_number_total             14270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05287j2.cif
_cod_data_source_block           sv0952a
_cod_database_code               7129244
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.468
_shelx_estimated_absorpt_t_min   0.335
_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. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(C57)
Uanis(C58) = Uanis(C59)
3. Rigid body (RIGU) restrains
 C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
 C60, C59, C58, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21),
 C23(H23), C24(H24), C25(H25), C26(H26), C35(H35), C36(H36), C37(H37), C39(H39),
  C40(H40), C41(H41), C42(H42)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              94969
_shelx_hkl_checksum              17256
_shelx_fab_checksum              47298
_olex2_submission_special_instructions 'No special instructions were received'