The origin of supramolecular chirality in 1-ferrocenyl amino acids.
Zong, Zhaohui; Zhang, Heng; Hao, Aiyou; Xing, Pengyao; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9695–9699; doi:10.1039/d1dt01905h

data_7707769
_publ_section_title
;
 The origin of supramolecular chirality in 1-ferrocenyl amino acids.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9695
_journal_page_last               9699
_journal_paper_doi               10.1039/d1dt01905h
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C14 H15 Fe N O3'
_chemical_formula_sum            'C14 H15 Fe N O3'
_chemical_formula_weight         301.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-05 deposited with the CCDC.	2021-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.299(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9913(2)
_cell_length_b                   9.9535(2)
_cell_length_c                   29.2374(6)
_cell_measurement_reflns_used    7850
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0170
_cell_measurement_theta_min      2.9970
_cell_volume                     2884.05(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     62.00 113.00   1.00    3.50    --  106.49-126.00 163.00   51
  2  \w     55.00  81.00   1.00    0.32    --   48.32-126.00 163.00   26
  3  \w     34.00  66.00   1.00    3.50    --  106.49 -57.00 120.00   32
  4  \w     34.00  96.00   1.00    3.50    --  106.49 -99.00  60.00   62
  5  \w     90.00 125.00   1.00    3.50    --  106.49-144.00  -5.00   35
  6  \w     63.00  88.00   1.00    0.32    --   48.32-144.00  -5.00   25
  7  \w     34.00 106.00   1.00    3.50    --  106.49 -99.00   0.00   72
  8  \w     38.00 110.00   1.00    3.50    --  106.49-125.00   0.00   72
  9  \w     40.00  66.00   1.00    3.50    --  106.49 -57.00 -30.00   26
 10  \w     34.00 111.00   1.00    3.50    --  106.49-125.00 -90.00   77
 11  \w     34.00 105.00   1.00    3.50    --  106.49 -77.00-180.00   71
 12  \w     98.00 178.00   1.00    3.50    --  106.49  38.00 -30.00   80
 13  \w     96.00 141.00   1.00    3.50    --  106.49 126.00-120.00   45
 14  \w    138.00 168.00   1.00    3.50    --  106.49 125.00-180.00   30
 15  \w     95.00 133.00   1.00    3.50    --  106.49 125.00-180.00   38
 16  \w     84.00 176.00   1.00    3.50    --  106.49  77.00 -60.00   92
 17  \w     93.00 178.00   1.00    3.50    --  106.49  38.00-120.00   85
 18  \w     84.00 141.00   1.00    3.50    --  106.49 144.00  48.00   57
 19  \w    -27.00  27.00   1.00    0.32    --  -48.32  19.00   0.00   54
 20  \w    -26.00  23.00   1.00    0.32    --  -48.32  19.00  90.00   49
 21  \w    -42.00 -13.00   1.00    3.50    --  -86.25  38.00  90.00   29
 22  \w    -43.00 -18.00   1.00    3.50    --  -86.25  38.00 120.00   25
 23  \w    -42.00 -13.00   1.00    3.50    --  -86.25  38.00  60.00   29
 24  \w    -91.00 -66.00   1.00    3.50    --  -86.25 144.00  48.00   25
 25  \w    -85.00 -41.00   1.00    0.32    --  -48.32 126.00-120.00   44
 26  \w    -80.00 -54.00   1.00    3.50    --  -86.25 126.00-120.00   26
 27  \w    -43.00 -13.00   1.00    3.50    --  -86.25  38.00-120.00   30
 28  \w   -120.00 -26.00   1.00    0.32    --  -48.32 -77.00  60.00   94
 29  \w   -119.00 -73.00   1.00    0.32    --  -48.32-126.00 163.00   46
 30  \w   -120.00 -61.00   1.00    0.32    --  -48.32-144.00  -5.00   59
 31  \w   -131.00-106.00   1.00    3.50    --  -86.25-144.00  -5.00   25
 32  \w   -115.00 -90.00   1.00    3.50    --  -86.25-126.00 163.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035869000
_diffrn_orient_matrix_UB_12      0.1438634000
_diffrn_orient_matrix_UB_13      0.0194816000
_diffrn_orient_matrix_UB_21      0.0195466000
_diffrn_orient_matrix_UB_22      0.0559286000
_diffrn_orient_matrix_UB_23      -0.0478345000
_diffrn_orient_matrix_UB_31      -0.1542515000
_diffrn_orient_matrix_UB_32      0.0105445000
_diffrn_orient_matrix_UB_33      -0.0123899000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14670
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.030
_diffrn_reflns_theta_max         67.030
_diffrn_reflns_theta_min         3.048
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 1922 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_coef       0.00015(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5062
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0554P)^2^+2.8163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                4603
_reflns_number_total             5062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01905h2.cif
_cod_data_source_block           200717d
_cod_depositor_comments
;
Adding full bibliography for 7707767--7707769.cif.

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C28 H30 Fe2 N2 O6'
_cod_original_formula_weight         602.24
_cod_original_formula_moiety         '2(C14 H15 Fe N O3)'
_cod_original_formula_units_Z            4
_cod_database_code               7707769
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         FeC
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.678
_diffrn_oxdiff_digest_frames
;
012b2bf108debe2bb154b93269fa3cb42601536ecae
;
_diffrn_oxdiff_digest_hkl
;
012a515f0a2c2f4d39cb879d5eb0b6f4dac9a1
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H26 of O26, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H12 of O12
2.a Riding coordinates:
 O26(H26)
2.b Ternary CH refined with riding coordinates:
 C23(H23), C10(H10)
2.c Aromatic/amide H refined with riding coordinates:
 N9(H9), N22(H22), C32(H32), C30(H30), C37(H37), C6(H6), C7(H7), C20(H20),
 C35(H35), C19(H19), C4(H4), C33(H33), C5(H5), C17(H17), C38(H38), C36(H36),
 C18(H18), C31(H31), C34(H34), C29(H29)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C27(H27A,H27B,H27C)
2.e Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_shelx_res_checksum              78924
_shelx_hkl_checksum              27165
_shelx_fab_checksum              98349
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.085
_oxdiff_exptl_absorpt_empirical_full_min 0.474