Neutral ligand TIPA-based two 2D metal-organic frameworks: ultrahigh selectivity of C2H2/CH4 and efficient sensing and sorption of Cr(VI)
Fu, Hong-Ru; Zhao, Ying; zhou, zhan; Yang, Xiao-Gang; ma, lufang; Dalton Transactions  (2018) –; doi:10.1039/C8DT00206A

data_7045500
_publ_section_title
;
 Neutral ligand TIPA-based two 2D metal-organic frameworks: ultrahigh
 selectivity of C2H2/CH4 and efficient sensing and sorption of Cr(VI)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT00206A
_journal_year                    2018
_chemical_formula_moiety         'C29 H25 N7 Ni O5, H2 O'
_chemical_formula_sum            'C29 H24.5 N7 Ni O6'
_chemical_formula_weight         625.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-29 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.810(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2283(9)
_cell_length_b                   15.0673(10)
_cell_length_c                   25.829(2)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    287.4(4)
_cell_measurement_theta_max      23.3590
_cell_measurement_theta_min      3.8370
_cell_volume                     3549.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      287.4(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -83.00  11.00   1.00   35.00    --  -15.84 -77.00 120.00   94
  2  \w    -29.00  49.00   1.00   35.00    --  -15.84  57.00-180.00   78
  3  \w    -85.00  -4.00   1.00   35.00    --  -15.84 -38.00-150.00   81
  4  \w    -64.00 -28.00   1.00   35.00    --  -15.84 115.00 155.53   36
  5  \w    -70.00  -7.00   1.00   35.00    --  -15.84 -57.00   0.00   63
  6  \w    -35.00  52.00   1.00   35.00    --  -15.84  38.00  30.00   87
  7  \w    -60.00  -1.00   1.00   35.00    --  -15.84 -57.00 -90.00   59
  8  \w    -29.00  51.00   1.00   35.00    --  -15.84  57.00 -90.00   80
  9  \w    -15.00  56.00   1.00   35.00    --   16.78 -99.00 120.00   71
 10  \w     15.00  64.00   1.00   35.00    --   16.78-113.00   5.73   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195847000
_diffrn_orient_matrix_UB_12      0.0387644000
_diffrn_orient_matrix_UB_13      0.0150377000
_diffrn_orient_matrix_UB_21      -0.0749999000
_diffrn_orient_matrix_UB_22      0.0079308000
_diffrn_orient_matrix_UB_23      0.0015190000
_diffrn_orient_matrix_UB_31      0.0064568000
_diffrn_orient_matrix_UB_32      -0.0255263000
_diffrn_orient_matrix_UB_33      0.0233154000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23610
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.192
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 1539 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4785
_reflns_number_total             6231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00206a2.cif
_cod_data_source_block           exp_1068
_cod_original_formula_sum        'C29 H24.50 N7 Ni O6'
_cod_database_code               7045500
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.901
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2-C28
 1.24 with sigma of 0.01
 C28-O3
 1.24 with sigma of 0.01
 C29-O4
 1.24 with sigma of 0.01
 C29-O5
 1.24 with sigma of 0.01
 O4-O5 \\sim O2-O3
 with sigma of 0.02
3. Rigid bond restraints
 O2, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Free rotating group:
 O6(H6A,H6B)
5.b Rotating group:
 O1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
;
_olex2_date_sample_data_collection 2018-01-28
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.911
_oxdiff_exptl_absorpt_empirical_full_min 0.451