An unusual porous cationic metal-organic framework based on a tetranuclear hydroxyl-copper(ii) cluster for fast and highly efficient dichromate trapping through a single-crystal to single-crystal process.
Lv, Xiu-Xiu; Shi, Lu-Lu; Li, Ke; Li, Bao-Long; Li, Hai-Yan; Chemical communications (Cambridge, England) 53 (2017) 1860–1863; doi:10.1039/c6cc09676j

data_7119434
_publ_section_title
;
 An unusual porous cationic metal-organic framework based on a
 tetranuclear hydroxyl-copper(ii) cluster for fast and highly efficient
 dichromate trapping through a single-crystal to single-crystal process.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1860
_journal_page_last               1863
_journal_paper_doi               10.1039/c6cc09676j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'0.5(C88 H84 Cu8 N24 O20), 2(Cr O3.5), 2(H2 O), 4(O1)'
_chemical_formula_sum            'C44 H54 Cr2 Cu4 N12 O23'
_chemical_formula_weight         1477.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-07-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_audit_update_record
;
2016-11-29 deposited with the CCDC.
2017-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.891(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6691(3)
_cell_length_b                   17.4598(5)
_cell_length_c                   20.4487(6)
_cell_measurement_reflns_used    7733
_cell_measurement_temperature    223.01(10)
_cell_measurement_theta_max      28.7350
_cell_measurement_theta_min      3.0270
_cell_volume                     3439.59(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      223.01(10)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -76.00   28.00   1.0000   31.9900
omega____ theta____ kappa____ phi______ frames
    -       13.6514    0.0000 -150.0000 104

  2 omega   13.00   40.00   1.0000   31.9900
omega____ theta____ kappa____ phi______ frames
    -       13.6514  -99.0000  -30.0000 27

  3 omega  -16.00   81.00   1.0000   31.9900
omega____ theta____ kappa____ phi______ frames
    -       13.6514   57.0000 -150.0000 97

  4 omega    1.00   26.00   1.0000   31.9900
omega____ theta____ kappa____ phi______ frames
    -      -14.5889  -99.0000 -180.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0103849000
_diffrn_orient_matrix_UB_12      0.0395600000
_diffrn_orient_matrix_UB_13      -0.0058274000
_diffrn_orient_matrix_UB_21      -0.0728766000
_diffrn_orient_matrix_UB_22      0.0055531000
_diffrn_orient_matrix_UB_23      -0.0041300000
_diffrn_orient_matrix_UB_31      -0.0006638000
_diffrn_orient_matrix_UB_32      0.0074467000
_diffrn_orient_matrix_UB_33      0.0340672000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18171
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6038
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0990P)^2^+12.8430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5011
_reflns_number_total             6038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09676j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7119434--7119435.cif.'
_cod_database_code               7119434
_chemical_oxdiff_formula         'C H O N'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 O(H,H) groups
2. Restrained distances
 H5-O5
 0.85 with sigma of 0.02
3. Rigid bond restraints
 Cu2, O4
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
Uanis(O7A) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O16)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O17) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: Cr1(0.5) Cr2(0.5) O12(0.5) O13(0.5) O14(0.4) O15(0.5) O16(0.25)
 O17(0.25) O18(0.5) O19(0.3) O20(0.3) O9(0.35) O8(0.25) O7A(0.25) O10(0.35)
 O7(0.5) O11(0.3)
6.a Free rotating group:
 O6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B), C14(H14A,H14B), C21(H21A,H21B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5A), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C16(H16),
  C17(H17), C19(H19), C20(H20)
;
_shelx_res_checksum              24039
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'