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_7240248
_publ_section_title
;
 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             2020-01-29
_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                   9.4529(6)
_cell_length_b                   26.3871(10)
_cell_length_c                   11.1375(6)
_cell_measurement_reflns_used    10108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0630
_cell_measurement_theta_min      4.1820
_cell_volume                     2778.1(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 0.994
_diffrn_measured_fraction_theta_max 0.941
_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    -61.00 -36.00   0.50   63.66    --   -0.00 -34.00 115.00   50
  2  \w    -76.00  28.00   0.50   63.66    --   -0.00 -77.00 -60.00  208
  3  \w    -15.00  60.00   0.50   63.66    --   -0.00  38.00   0.00  150
  4  \w    -40.00 -15.00   0.50   63.66    --   -0.00 -82.00-120.00   50
  5  \w     46.00  71.00   0.50   63.66    --   -0.00  57.00-180.00   50
  6  \w     22.00  52.00   0.50   63.66    --   -0.00  57.00 150.00   60
  7  \w     36.00  61.00   0.50   63.66    --   -0.00  57.00-120.00   50
;
_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      0.0562808000
_diffrn_orient_matrix_UB_12      -0.0135607000
_diffrn_orient_matrix_UB_13      0.0272551000
_diffrn_orient_matrix_UB_21      0.0382139000
_diffrn_orient_matrix_UB_22      0.0229342000
_diffrn_orient_matrix_UB_23      0.0070811000
_diffrn_orient_matrix_UB_31      -0.0315676000
_diffrn_orient_matrix_UB_32      0.0036264000
_diffrn_orient_matrix_UB_33      0.0571410000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36655
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.236
_diffrn_reflns_theta_min         3.766
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86257
_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    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.4779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.890
_reflns_number_gt                6714
_reflns_number_total             7626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00262c2.cif
_cod_data_source_block           1-D
_cod_database_code               7240248
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHONCu
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.850
_reflns_odcompleteness_completeness 99.48
_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), C5(H5A,H5B), C4(H4A,H4B), C27(H27A,H27B), C25(H25A,H25B)
2.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C17(H17), C18(H18), C9(H9), C15(H15), C14(H14), C21(H21), C11(H11),
 C23(H23), C20(H20), C8(H8), C12(H12), C24(H24)
2.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_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 1.423
_oxdiff_exptl_absorpt_empirical_full_min 0.738