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_7055217
_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                   15.7377(5)
_cell_length_b                   21.1254(8)
_cell_length_c                   11.7487(3)
_cell_measurement_reflns_used    4951
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6910
_cell_measurement_theta_min      4.2950
_cell_volume                     3906.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0466
_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       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10122
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.984
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58968
_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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.976
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 2111 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6524
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0717P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.819
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                5894
_reflns_number_total             6524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02236c2.cif
_cod_data_source_block           1-d
_cod_depositor_comments
'Adding full bibliography for 7055217--7055218.cif.'
_cod_original_formula_sum        'C29 H22 Cd1.50 N4 O7'
_cod_database_code               7055217
_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
 C24B-C23B = C24A-C23A = C24A-C20 = C24B-C20 = C21A-C20 = C21B-C20 = C22A-C21A
 = C22B-C21B
 1.4 with sigma of 0.01
 N3-C23B = N3-C23A = N3-C22A = N3-C22B
 1.33 with sigma of 0.01
3. Restrained planarity
 N3, C20, C21A, C24A, C23A, C22A
 with sigma of 0.1
 N3, C20, C22B, C21B, C24B, C23B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N3 \\sim C20 \\sim C21A \\sim C24A \\sim C23A \\sim C22A \\sim C22B \\sim C21B
\\sim C24B \\sim C23B: 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(0.73714) H21A(0.73714) C24A(0.73714) H24A(0.73714)
 C23A(0.73714) H23A(0.73714) C22A(0.73714) H22A(0.73714) C22B(0.26286)
 H22B(0.26286) C21B(0.26286) H21B(0.26286) C24B(0.26286) H24B(0.26286)
 C23B(0.26286) H23B(0.26286) H3AA(0.75) H3AB(0.75) H3BC(0.25) H3BD(0.25)
 H5AA(0.75) H5AB(0.75) H5BC(0.25) H5BD(0.25) C4A(0.75) H4AA(0.75) H4AB(0.75)
 C4B(0.25) H4BA(0.25) H4BB(0.25)
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:
 C19(H19), C30(H30), C29(H29), C15(H15), C18(H18), C25(H25), C21A(H21A),
 C24A(H24A), C23A(H23A), C22A(H22A), C22B(H22B), C21B(H21B), C24B(H24B),
 C23B(H23B), C26(H26), C16(H16), C10(H10), C12(H12), C8(H8)
;
_shelx_res_checksum              6396
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'