Cluster- and chain-based magnetic MOFs derived from 3d metal ions and 1,3,5-benzenetricarboxylate
Liu, Sui-Jun; Han, Song-De; Chang, Ze; Bu, Xian-He; New J. Chem. 40 (2016) 2680–; doi:10.1039/C5NJ02161H

data_7055321
_publ_section_title
;
 Cluster- and chain-based magnetic MOFs derived from 3d metal ions and
 1,3,5-benzenetricarboxylate
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2680
_journal_paper_doi               10.1039/C5NJ02161H
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety
'0.5(C104 H124 Co12 N8 Na4 O72), C4 H9 N O, 2(H2 O)'
_chemical_formula_sum            'C56 H75 Co6 N5 Na2 O39'
_chemical_formula_weight         1841.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2015-11-26 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1249(7)
_cell_length_b                   12.1064(5)
_cell_length_c                   17.7333(7)
_cell_measurement_reflns_used    18461
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.4
_cell_volume                     3715.1(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.1461
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19250
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.366
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 2438 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8441
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0740
_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^)+(0.0670P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                7085
_reflns_number_total             8441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02161h2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055321--7055323.cif.
;
_cod_database_code               7055321
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H19A,H19B} of O19
 At 1.5 times of:
  All C(H,H,H) groups, {H20A,H20B} of O20, {H14A,H14B} of O14, All O(H,H,H)
  groups
2. Restrained distances
 H20A-O4_$1
 2.1 with sigma of 0.02
 O13-H13
 0.82 with sigma of 0.02
3. Restrained planarity
 O17, N3, C27, C28, C29, C30
 with sigma of 0.1
4. Rigid bond restraints
 O15, N1, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O16, N2, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O16, N2, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O17, N3, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Others
 Fixed Sof: O17(0.5) N3(0.5) C27(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
7.a Riding coordinates:
 O19(H19A,H19B), O20(H20A,H20B), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C),
 O18(H18A,H18B)
7.b Rotating group:
 O14(H14A,H14B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C13(H13A), C15(H15)
7.d Idealised Me refined as rotating group:
 C20(H20C,H20D,H20E), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'