Fabrication of zinc-dicarboxylate- and zinc-pyrazolate-carboxylate-framework thin films through vapour-solid deposition.
Medishetty, Raghavender; Zhang, Zongji; Sadlo, Alexander; Cwik, Stefan; Peeters, Daniel; Henke, Sebastian; Mangayarkarasi, Nagarathinam; Devi, Anjana; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14179–14183; doi:10.1039/c8dt00352a

data_7046248
_publ_section_title
;
 Fabrication of zinc-dicarboxylate- and
 zinc-pyrazolate-carboxylate-framework thin films through vapour-solid
 deposition.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14179
_journal_page_last               14183
_journal_paper_doi               10.1039/c8dt00352a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'0.25(C128 H64 O64 Zn12), 1.4(H2 O), 2(C2 H8 N)'
_chemical_formula_sum            'C36 H34.8 N2 O17.4 Zn3'
_chemical_formula_weight         969.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1m3mfs
_audit_creation_date             2018-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-04-23 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9516(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.1191(7)
_cell_length_b                   9.72325(14)
_cell_length_c                   18.2372(3)
_cell_measurement_reflns_used    33918
_cell_measurement_temperature    112(3)
_cell_measurement_theta_max      76.2330
_cell_measurement_theta_min      4.7090
_cell_volume                     5850.92(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -68.00   35.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302   38.0000  120.0000 103

  2 omega -115.00  -12.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000  -30.0000 103

  3 omega -124.00  -79.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000   30.0000 45

  4 omega    2.00   99.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000 -180.0000 97

  5 omega    2.00   99.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000  -30.0000 97

  6 omega  -33.00   71.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -57.0000 -150.0000 104

  7 omega   35.00   69.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 34

  8 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   90.0000 75

  9 omega   35.00  150.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -120.0000 115

 10 omega   35.00  116.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -150.0000 81

 11 omega   35.00   69.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 34

 12 omega   30.00  110.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -97.0000  -71.0000 80

 13 omega   38.00   77.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 39

 14 omega   35.00   69.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 34

 15 omega   35.00  116.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   90.0000 81

 16 omega   34.00  147.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -120.0000 113

 17 omega   35.00  116.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   30.0000 81

 18 omega   35.00  116.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 81

 19 omega   82.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   60.0000 76

 20 omega   30.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000   30.0000 128

 21 omega   39.00  143.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000    0.0000 104

 22 omega   35.00   69.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 34

 23 omega   35.00   69.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 34

 24 omega   30.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  150.0000 128

 25 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000  -30.0000 112

 26 omega -115.00  -12.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000  150.0000 103

 27 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000  120.0000 112

 28 omega  -68.00   35.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302   38.0000   60.0000 103

 29 omega -115.00  -12.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000 -120.0000 103

 30 omega -124.00  -79.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000 -150.0000 45

 31 omega -115.00  -12.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000   60.0000 103

 32 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000 -150.0000 112

 33 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 75

 34 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 79

 35 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -30.0000 79

 36 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 75

 37 omega   82.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -60.0000 76

 38 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -60.0000 79

 39 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -150.0000 75

 40 omega   82.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -180.0000 76

 41 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -90.0000 79

 42 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000    0.0000 75

 43 omega   82.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -120.0000 76

 44 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  150.0000 79

 45 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 79

 46 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   90.0000 79

 47 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   60.0000 75

 48 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 75

 49 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000 -120.0000 112

 50 omega -117.00  -15.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -38.0000    0.0000 102

 51 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000  -60.0000 112

 52 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000   60.0000 112

 53 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000    0.0000 112

 54 omega -120.00   -8.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000   90.0000 112

 55 omega -117.00  -15.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -38.0000   60.0000 102

 56 omega   -5.00  123.00   1.0000    4.1150
omega____ theta____ kappa____ phi______ frames
    -       41.2302   19.0000  -90.0000 128

 57 omega   83.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 75

 58 omega   79.00  158.00   1.0000   16.4550
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  120.0000 79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0222297000
_diffrn_orient_matrix_UB_12      0.1392726000
_diffrn_orient_matrix_UB_13      -0.0064696000
_diffrn_orient_matrix_UB_21      -0.0384641000
_diffrn_orient_matrix_UB_22      -0.0683187000
_diffrn_orient_matrix_UB_23      0.0249884000
_diffrn_orient_matrix_UB_31      0.0143334000
_diffrn_orient_matrix_UB_32      0.0322978000
_diffrn_orient_matrix_UB_33      0.0807727000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63898
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.817
_diffrn_reflns_theta_min         4.741
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.1918
_exptl_crystal_size_mid          0.1861
_exptl_crystal_size_min          0.0844
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+5.5339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5830
_reflns_number_total             6107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00352a2.cif
_cod_data_source_block           mr_zzj_24_red_abs
_cod_depositor_comments          'Adding full bibliography for 7046248.cif.'
_cod_original_cell_volume        5850.94(18)
_cod_original_formula_sum        'C36 H34.80 N2 O17.40 Zn3'
_cod_database_code               7046248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn3 C39 H46 N4 O18'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C1A-C2A
 2.5 with sigma of 0.01
 C1B-C2B
 2.5 with sigma of 0.01
 C1A-C2A \\sim C1B-C2B
 with sigma of 0.04
 N1A-C1A \\sim N1B-C1B
 with sigma of 0.02
 N1A-C2A \\sim N1B-C2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1A \\sim N1B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 N1A, C1A, C2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1B, C1B, C2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O1W(0.7) H1WA(0.7) H1WB(0.7) N1A(0.7) H1AA(0.7) H1AB(0.7) N1B(0.3)
 H1BA(0.3) H1BB(0.3) C1A(0.7) H1AC(0.7) H1AD(0.7) H1AE(0.7) C1B(0.3) H1BC(0.3)
 H1BD(0.3) H1BE(0.3) C2A(0.7) H2AA(0.7) H2AB(0.7) H2AC(0.7) C2B(0.3) H2BA(0.3)
 H2BB(0.3) H2BC(0.3)
6.a Free rotating group:
 O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N1B(H1BA,H1BB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C15(H15), C16(H16)
6.d Idealised Me refined as rotating group:
 C1A(H1AC,H1AD,H1AE), C1B(H1BC,H1BD,H1BE), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,
 H2BC)
;
_olex2_submission_special_instructions 'No special instructions were received'