Four new metal-organic frameworks based on diverse secondary building units: sensing and magnetic properties.
Yan, Yang-Tian; Zhang, Wen-Yan; Zhang, Fang; Cao, Feng; Yang, Rui-Feng; Wang, Yao-Yu; Hou, Lei; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1682–1692; doi:10.1039/c7dt04696k

data_7045167
_publ_section_title
;
 Four new metal-organic frameworks based on diverse secondary building
 units: sensing and magnetic properties.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1682
_journal_page_last               1692
_journal_paper_doi               10.1039/c7dt04696k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.25(C92 H80 O64 Zn12), C5 H9 N O, 2(H2 O)'
_chemical_formula_sum            'C28 H33 N O19 Zn3'
_chemical_formula_weight         883.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6370(10)
_cell_length_b                   20.398(2)
_cell_length_c                   18.307(2)
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.36
_cell_volume                     3225.3(6)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15434
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         1.997
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0972 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.6976.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         3037
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0470P)^2^+25.5976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2923
_reflns_number_total             3037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04696k1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045167--7045170.cif.'
_cod_original_cell_volume        3225.3(7)
_cod_database_code               7045167
_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) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Zn1A) \\sim Ueq, Uanis(Zn1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O12, C14, N2, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, Zn1A, Zn1, O7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Zn1A)=1-FVAR(1)
 Sof(Zn1)=FVAR(1)
 Sof(O7A)=1-FVAR(2)
 Sof(O7)=FVAR(2)
 Fixed Sof: O12(0.5) C14(0.5) N2(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) O13(0.5) H13A(0.5) H13B(0.5) O14(0.5) H14A(0.5) H14B(0.5)
6.a Riding coordinates:
 O8(H8), O9(H9A,H9B), O7(H7A,H7B), O13(H13A,H13B), O14(H14A,H14B)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C6(H6), C3(H3), C5(H5)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              3547
_shelx_hkl_checksum              29089
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'