From coordination polymers to nanocrystals: general and facile synthesis of ultra-small metal oxide nanocrystals.
Zhang, Jiajia; Cui, Fang; Li, Li; Liu, Yang; Zhang, Xiao; Cui, Tieyu; Chemical communications (Cambridge, England) 56 (2020) 6145–6148; doi:10.1039/d0cc01248c

data_7126451
_publ_section_title
;
 From coordination polymers to nanocrystals: general and facile synthesis
 of ultra-small metal oxide nanocrystals.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6145
_journal_page_last               6148
_journal_paper_doi               10.1039/d0cc01248c
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H20 O8 Zn2'
_chemical_formula_sum            'C16 H20 O8 Zn2'
_chemical_formula_weight         471.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2018-09-03 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8332(5)
_cell_length_b                   9.0061(2)
_cell_length_c                   13.2032(3)
_cell_measurement_reflns_used    2403
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8547
_cell_measurement_theta_min      2.7322
_cell_volume                     2120.53(9)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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_detector_area_resol_mean 15.9737
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -32.00   79.00   1.0000   14.3400
omega____ theta____ kappa____ phi______ frames
    -       20.8282  -19.0000   90.0000 111

  2 omega   49.00   74.00   1.0000   14.3400
omega____ theta____ kappa____ phi______ frames
    -       20.8282  178.0000  -30.0000 25

  3 omega  -22.00    8.00   1.0000   14.3400
omega____ theta____ kappa____ phi______ frames
    -      -21.0626  -37.0000  -30.0000 30

  4 omega  -99.00  -74.00   1.0000   14.3400
omega____ theta____ kappa____ phi______ frames
    -      -21.0626 -178.0000   90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0279479000
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_diffrn_orient_matrix_UB_13      0.0175326000
_diffrn_orient_matrix_UB_21      -0.0264593000
_diffrn_orient_matrix_UB_22      -0.0586934000
_diffrn_orient_matrix_UB_23      -0.0007364000
_diffrn_orient_matrix_UB_31      0.0100628000
_diffrn_orient_matrix_UB_32      -0.0162688000
_diffrn_orient_matrix_UB_33      -0.0508143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5890
_diffrn_reflns_point_group_measured_fraction_full 0.776
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        25.093
_diffrn_reflns_theta_max         25.093
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 759 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2930
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.484
_reflns_Friedel_fraction_full    0.531
_reflns_Friedel_fraction_max     0.531
_reflns_number_gt                2604
_reflns_number_total             2930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01248c2.cif
_cod_data_source_block           pna21
_cod_depositor_comments          'Adding full bibliography for 7126451.cif.'
_cod_database_code               7126451
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.657
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a X=CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C11(H11A,H11B), C25(H25A,H25B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              27704
_shelx_hkl_checksum              22366
_olex2_submission_special_instructions 'No special instructions were received'