A unique zinc-organic framework constructed through in situ ligand synthesis for conversion of CO2 under mild conditions and luminescent sensor for Cr2O72-/CrO42-
Song, Tian-Qun; Dong, Jie; Gao, Hong-Ling; Cui, Jian-zhong; Zhao, Bin; Dalton Trans.  (2017) –; doi:10.1039/C7DT02819A

data_7044232
_publ_section_title
;
 A unique zinc-organic framework constructed through in situ ligand
 synthesis for conversion of CO2 under mild conditions and luminescent
 sensor for Cr2O72-/CrO42-
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02819A
_journal_year                    2017
_chemical_formula_moiety         '0.5(C12 H20 N16 O16 Zn6)'
_chemical_formula_sum            'C6 H10 N8 O8 Zn3'
_chemical_formula_weight         518.33
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-09-11 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.645(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.5917(11)
_cell_length_b                   14.645(3)
_cell_length_c                   6.4975(11)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.5570
_cell_measurement_theta_min      3.0300
_cell_volume                     717.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  53.00   1.00    3.50    --  -19.25  37.00  30.00   73
  2  \w     14.00  53.00   1.00    3.50    --  -19.25  37.00  90.00   39
  3  \w     35.00  95.00   1.00    3.50    --   18.94 178.00-120.00   60
  4  \w    -84.00 -51.00   1.00    3.50    --  -19.25-178.00 120.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0223104000
_diffrn_orient_matrix_UB_12      0.0399116000
_diffrn_orient_matrix_UB_13      -0.0528965000
_diffrn_orient_matrix_UB_21      -0.0529170000
_diffrn_orient_matrix_UB_22      -0.0152316000
_diffrn_orient_matrix_UB_23      -0.0906679000
_diffrn_orient_matrix_UB_31      -0.0744191000
_diffrn_orient_matrix_UB_32      0.0228547000
_diffrn_orient_matrix_UB_33      0.0326464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2468
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1263
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+3.8222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                987
_reflns_number_total             1263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02819a2.cif
_cod_data_source_block           p170324e4
_cod_database_code               7044232
_chemical_oxdiff_formula         'C N O Zn'
_chemical_oxdiff_usercomment     STQ-7
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9996(6)
 0.0004(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 H7b-O7
 0.85 with sigma of 0.02
 H3-O3
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 O3(H3), O7(H7a,H7b)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b)
;
_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 2.439
_oxdiff_exptl_absorpt_empirical_full_min 0.524