Salicylaldehydate coordinated two-dimensional-conjugated metal–organic frameworks
Mohammed, Abdul Khayum; Pena-Sánchez, Pilar; Pandikassala, Ajmal; Gaber, Safa; AlKhoori, Ayesha A.; Skorjanc, Tina; Polychronopoulou, Kyriaki; Kurungot, Sreekumar; Gándara, Felipe; Shetty, Dinesh; Chemical Communications 59 (2023) 2608–2611; doi:10.1039/D2CC06283F

data_7131254
_publ_section_title
;
 Salicylaldehydate coordinated two-dimensional-conjugated metal--organic
 frameworks
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2608
_journal_page_last               2611
_journal_paper_doi               10.1039/D2CC06283F
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H23 N2 O5 Zn, C2 H3 O2'
_chemical_formula_sum            'C14 H26 N2 O7 Zn'
_chemical_formula_weight         399.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1pz752
_audit_creation_date             2017-07-05
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:34:12, GUI svn.r4372)
;
_audit_update_record
;
2017-10-04 deposited with the CCDC.	2023-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.785(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0266(3)
_cell_length_b                   16.6464(9)
_cell_length_c                   9.3779(4)
_cell_measurement_reflns_used    2547
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.7880
_cell_measurement_theta_min      3.9920
_cell_volume                     932.13(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.6889
_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     34.00  71.00   1.00    2.40    --   19.75-178.00  90.00   37
  2  \w      4.00  48.00   1.00    2.40    --   19.75  57.00 -90.00   44
  3  \w    -51.00  92.00   1.00    2.40    --   19.75   0.00-150.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0651638000
_diffrn_orient_matrix_UB_12      0.0048459000
_diffrn_orient_matrix_UB_13      -0.0570571000
_diffrn_orient_matrix_UB_21      0.0805357000
_diffrn_orient_matrix_UB_22      0.0221359000
_diffrn_orient_matrix_UB_23      0.0462733000
_diffrn_orient_matrix_UB_31      0.0582028000
_diffrn_orient_matrix_UB_32      -0.0360468000
_diffrn_orient_matrix_UB_33      0.0208521000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4094
_diffrn_reflns_theta_full        28.87
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.3374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                3271
_reflns_number_total             3363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2cc06283f2.cif
_cod_data_source_block           zalagtm
_cod_depositor_comments
'Adding full bibliography for 7131251--7131256.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7131254
_chemical_oxdiff_formula         'C10 H10 N10 O10 Zn1'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, {H8A,H8B} of C8, H10 of C10, H6 of C6, {H14A,H14B} of C14, H9A of
  C9, H7 of C7, H9 of N9, H3 of C3
 At 1.5 times of:
  {H17A,H17B} of O17, {H16A,H16B} of O16, {H5A,H5B,H5C} of C5, {H15A,H15B} of
  O15, {H1A,H1B,H1C} of C1, {H21A,H21B,H21C} of C21
2.a Rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B)
2.b Ternary CH refined with riding coordinates:
 N9(H9), C10(H10), C9(H9A)
2.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C14(H14A,H14B)
2.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3)
2.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.796