A pair of homochiral porous metal‒organic frameworks with a helical metal-carboxylate layer
Xu, Zhong-Xuan; Liu, Liyang; Zhang, Jian; New J. Chem. 40 (2016) 1927–; doi:10.1039/C5NJ02236C

data_7055218
_publ_section_title
;
 A pair of homochiral porous metal--organic frameworks with a helical
 metal-carboxylate layer
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              1927
_journal_paper_doi               10.1039/C5NJ02236C
_journal_volume                  40
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C29 H22 Cd1.5 N4 O7'
_chemical_formula_sum            'C29 H22 Cd1.5 N4 O7'
_chemical_formula_weight         707.10
_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'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-24 deposited with the CCDC.
2015-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6969(6)
_cell_length_b                   20.9233(7)
_cell_length_c                   11.7168(4)
_cell_measurement_reflns_used    10223
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5480
_cell_measurement_theta_min      3.8110
_cell_volume                     3848.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18514
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.399
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction using spherical harmonics,implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2414 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6750
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0530P)^2^+1.2507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6157
_reflns_number_total             6750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02236c2.cif
_cod_data_source_block           1-L
_cod_depositor_comments
'Adding full bibliography for 7055217--7055218.cif.'
_cod_original_formula_sum        'C29 H22 Cd1.50 N4 O7'
_cod_database_code               7055218
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C24A-C20 \\sim C24B-C20 \\sim C21B-C20 \\sim C21A-C20
 with sigma of 0.01
 N3-C22B \\sim N3-C22A \\sim N3-C23A \\sim N3-C23B
 with sigma of 0.01
3. Restrained planarity
 C20, N3, C21A, C22A, C23A, C24A
 with sigma of 0.1
 C20, N3, C23B, C24B, C22B, C21B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C20 \\sim N3 \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C23B \\sim C24B
\\sim C22B \\sim C21B: within 2A with sigma of 0.003 and sigma for terminal
atoms of 0.006
Uanis(C4A) \\sim Ueq, Uanis(C4B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: C21A(0.72101) H21A(0.72101) C22A(0.72101) H22A(0.72101)
 C23A(0.72101) H23A(0.72101) C24A(0.72101) H24A(0.72101) C23B(0.27899)
 H23B(0.27899) C24B(0.27899) H24B(0.27899) C22B(0.27899) H22B(0.27899)
 C21B(0.27899) H21B(0.27899) H3AA(0.65) H3AB(0.65) H3BC(0.35) H3BD(0.35)
 H5AA(0.65) H5AB(0.65) H5BC(0.35) H5BD(0.35) C4A(0.65) H4AA(0.65) H4AB(0.65)
 C4B(0.35) H4BA(0.35) H4BB(0.35)
6.a Ternary CH refined with riding coordinates:
 C2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C5(H5AA,H5AB), C5(H5BC,H5BD), C4A(H4AA,H4AB),
 C4B(H4BA,H4BB)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C18(H18), C15(H15), C19(H19), C12(H12), C16(H16), C8(H8), C10(H10),
 C26(H26), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C23B(H23B),
 C24B(H24B), C22B(H22B), C21B(H21B), C29(H29), C30(H30)
;
_shelx_res_checksum              43563
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'