Semi-conductive helical homochiral metal−organic frameworks based on enantiomeric proline derivatives
Ma, Yu-Lu; Meng, Qin; Xu, Zhong-Xuan; CrystEngComm  (2020) –; doi:10.1039/D0CE00262C

data_7240247
_publ_section_title
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 Semi-conductive helical homochiral metal&#x2212;organic frameworks based
 on enantiomeric proline derivatives
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00262C
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C23 H19 Cu N3 O5, C5 H11 N O, H2 O'
_chemical_formula_sum            'C28 H32 Cu N4 O7'
_chemical_formula_weight         600.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-21 deposited with the CCDC.	2020-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4610(6)
_cell_length_b                   26.3464(13)
_cell_length_c                   11.1125(8)
_cell_measurement_reflns_used    6732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8240
_cell_measurement_theta_min      4.0100
_cell_volume                     2769.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.917
_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    -27.00  30.00   0.50  153.11    --   -0.00 -82.00  60.00  114
  2  \w    -51.00  -7.00   0.50  153.11    --   -0.00 -82.00 -90.00   88
  3  \w    -76.00 -49.00   0.50  153.11    --   -0.00 -77.00 -60.00   54
  4  \w    -29.00  -3.00   0.50  153.11    --   -0.00 -77.00 -60.00   52
  5  \w    -15.00  22.50   0.50  153.11    --   -0.00  37.00 -71.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0432616000
_diffrn_orient_matrix_UB_12      0.0190176000
_diffrn_orient_matrix_UB_13      -0.0261801000
_diffrn_orient_matrix_UB_21      0.0611497000
_diffrn_orient_matrix_UB_22      0.0141888000
_diffrn_orient_matrix_UB_23      -0.0151891000
_diffrn_orient_matrix_UB_31      0.0035361000
_diffrn_orient_matrix_UB_32      -0.0127208000
_diffrn_orient_matrix_UB_33      -0.0561703000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22502
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.198
_diffrn_reflns_theta_min         3.658
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       needle
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2404 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0526P)^2^+0.0927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.718
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.838
_reflns_number_gt                6351
_reflns_number_total             7267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00262c2.cif
_cod_data_source_block           1-L
_cod_database_code               7240247
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHONCu
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.729
_reflns_odcompleteness_completeness 99.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB)
2.b Ternary CH refined with riding coordinates:
 C2(H2)
2.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C25(H25A,H25B), C27(H27A,H27B)
2.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C23(H23), C22(H22), C9(H9), C14(H14), C21(H21), C8(H8),
 C15(H15), C11(H11), C17(H17), C12(H12), C28(H28)
2.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C24(H24A,H24B,H24C)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.470
_oxdiff_exptl_absorpt_empirical_full_min 0.394