A blessing and a curse: impact of urea derivatives on the secondary building unit of Ca-MOFs prepared in deep eutectic solvents.
Teixeira, Michaël; Louis, Benoît; Baudron, Stéphane A; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5006–5016; doi:10.1039/d4dt03254c

data_7718045
_publ_section_title
;
 A blessing and a curse: impact of urea derivatives on the secondary
 building unit of Ca-MOFs prepared in deep eutectic solvents.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5006
_journal_page_last               5016
_journal_paper_doi               10.1039/d4dt03254c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C13 H14 Ca N2 O5'
_chemical_formula_sum            'C13 H14 Ca N2 O5'
_chemical_formula_weight         318.34
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-11-19 deposited with the CCDC.	2025-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.263(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8758(3)
_cell_length_b                   13.2330(2)
_cell_length_c                   7.07730(10)
_cell_measurement_reflns_used    15404
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.6360
_cell_measurement_theta_min      1.9470
_cell_volume                     1387.30(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.70a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2930
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -112.00  82.00   1.00  100.00   6.00  21.32  40.00    --   194
  2  \f   -119.00 -11.00   1.00  100.00  37.00  21.32 -40.00    --   108
  3  \w    -14.00  56.00   1.00  100.00    --   21.32 -38.00-150.00   70
  4  \w    -38.00  56.00   1.00  100.00    --   21.32 -38.00 120.00   94
  5  \f    106.00 180.00   1.00  100.00 -37.70 -22.41 -40.00    --    74
  6  \w    -43.00   7.00   1.00  100.00    --  -22.41  40.00 -48.70   50
  7  \w   -112.00  10.00   1.00  100.00    --  -22.41 -40.00  57.50  122
  8  \f      2.00  99.00   1.00    1.00  47.65   0.00  20.00    --    97
  9  \w    -17.00  50.00   1.00    1.00    --    0.00  38.00-180.00   67
 10  \w    -17.00  98.00   1.00    1.00    --    0.00  38.00 -30.00  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0055220000
_diffrn_orient_matrix_UB_12      0.0442054000
_diffrn_orient_matrix_UB_13      -0.0442063000
_diffrn_orient_matrix_UB_21      0.0108877000
_diffrn_orient_matrix_UB_22      -0.0249618000
_diffrn_orient_matrix_UB_23      -0.0773939000
_diffrn_orient_matrix_UB_31      -0.0436864000
_diffrn_orient_matrix_UB_32      -0.0006595000
_diffrn_orient_matrix_UB_33      -0.0339695000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67199
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6821
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        23.778
_diffrn_reflns_theta_max         28.765
_diffrn_reflns_theta_min         1.951
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.70a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         6821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+0.4900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6193
_reflns_number_total             6821
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9739\% 
around [-0.19 -0.00 0.98] (reciprocal) or [0.00 0.00 1.00] (direct)
;
_cod_data_source_file            d4dt03254c2.cif
_cod_data_source_block           CaMOF8
_cod_depositor_comments
'Adding full bibliography for 7718045--7718055.cif.'
_cod_database_code               7718045
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C13 H14 N2 O5 Ca'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7694(8)
 0.2306(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), N1(H1), N2(H2)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              80151
_shelx_hkl_checksum              39066
_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 4.541
_oxdiff_exptl_absorpt_empirical_full_min 0.562
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2