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_7131252
_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         'C11 H13 Br Cd N2 O2, C H3'
_chemical_formula_sum            'C12 H16 Br Cd N2 O2'
_chemical_formula_weight         412.58
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1pz730
_audit_creation_date             2017-07-11
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.3028(8)
_cell_length_b                   16.3028(8)
_cell_length_c                   14.8888(5)
_cell_measurement_reflns_used    2347
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.0470
_cell_measurement_theta_min      3.8180
_cell_volume                     3427.0(3)
_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 0.9971
_diffrn_measured_fraction_theta_max 0.7245
_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     18.00  71.00   1.00   52.14    --   19.59  37.00  60.00   53
  2  \w     22.00  88.00   1.00   52.14    --   19.59  77.00 -60.00   66
;
_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      -0.0422305000
_diffrn_orient_matrix_UB_12      -0.0080754000
_diffrn_orient_matrix_UB_13      0.0215184000
_diffrn_orient_matrix_UB_21      0.0010825000
_diffrn_orient_matrix_UB_22      -0.0349153000
_diffrn_orient_matrix_UB_23      0.0275576000
_diffrn_orient_matrix_UB_31      0.0272190000
_diffrn_orient_matrix_UB_32      0.0351901000
_diffrn_orient_matrix_UB_33      0.0323293000
_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  0.1051
_diffrn_reflns_av_unetI/netI     0.1226
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7866
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         3.09
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57924
_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            white
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         4398
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0955
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2463
_refine_ls_wR_factor_ref         0.2990
_reflns_number_gt                2752
_reflns_number_total             4398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2cc06283f2.cif
_cod_data_source_block           brcala
_cod_depositor_comments
'Adding full bibliography for 7131251--7131256.cif.'
_cod_original_cell_volume        3427.0(4)
_cod_database_code               7131252
_chemical_oxdiff_formula         'C10 H10 N10 O10 Br1 Cd1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H2 of C2, H5 of C5, {H14A,H14B} of C14, H10 of C10, H6 of C6, {H8A,H8B} of
  C8, H3 of C3, H1 of C1
 At 1.5 times of:
  {H4A,H4B,H4C} of C4, {H9A,H9B,H9C} of C9
2.a Ternary CH refined with riding coordinates:
 C10(H10), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C1(H1)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.940
_oxdiff_exptl_absorpt_empirical_full_min 0.593