Investigation of the preparation and reactivity of metal-organic frameworks of cerium and pyridine-2,4,6-tricarboxylate.
Fonseca de Lima, Juliana; Moreno, Fernanda V. S.; Menezes, Bruno A. T.; da Silva Barbosa, Jader; Waddington, Matthew C.; Franklin, Siân A; Clarkson, Guy J.; Walker, Marc; Serra, Osvaldo A.; Walton, Richard I.; Dalton transactions (Cambridge, England : 2003) 51 (2021) 145–155; doi:10.1039/d1dt03514b

data_7709038
_publ_section_title
;
 Investigation of the preparation and reactivity of metal-organic
 frameworks of cerium and pyridine-2,4,6-tricarboxylate.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              145
_journal_page_last               155
_journal_paper_doi               10.1039/d1dt03514b
_journal_volume                  51
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H11 Ce N2 O8, H2 O'
_chemical_formula_sum            'C11 H13 Ce N2 O9'
_chemical_formula_weight         457.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.062(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8285(3)
_cell_length_b                   10.1903(9)
_cell_length_c                   9.1832(3)
_cell_measurement_reflns_used    7899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2000
_cell_measurement_theta_min      3.9860
_cell_volume                     1481.22(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.913
_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    -29.00  92.00   1.00   14.00    --   11.87  19.00 -60.00  121
  2  \w    -63.00  36.00   1.00   14.00    --   11.87 -37.00 120.00   99
  3  \w    -39.00 -14.00   1.00   14.00    --  -10.70  57.00-150.00   25
  4  \w    -20.00  30.00   1.00   14.00    --  -10.70 -99.00 -60.00   50
  5  \w    -83.00  17.00   1.00   14.00    --  -10.70 -57.00  60.00  100
  6  \w     34.00  99.00   1.00   14.00    --   11.87-178.00 120.00   65
  7  \w     34.00  99.00   1.00   14.00    --   11.87-178.00   0.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0576734000
_diffrn_orient_matrix_UB_12      -0.0289197000
_diffrn_orient_matrix_UB_13      0.0546367000
_diffrn_orient_matrix_UB_21      0.0157110000
_diffrn_orient_matrix_UB_22      -0.0769905000
_diffrn_orient_matrix_UB_23      0.0087430000
_diffrn_orient_matrix_UB_31      0.0489165000
_diffrn_orient_matrix_UB_32      -0.0094793000
_diffrn_orient_matrix_UB_33      0.0615677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10412
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.715
_diffrn_reflns_theta_min         3.251
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 1578 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).

Hooft y: -0.012(7) Olex2
Flack x: -0.028(7) Shelx 2016
;
_refine_ls_abs_structure_Flack   -0.028(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0169
_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^)+(0.0165P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0363
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.791
_reflns_number_gt                3501
_reflns_number_total             3584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03514b2.cif
_cod_data_source_block           fvs3
_cod_depositor_comments
'Adding full bibliography for 7709038--7709041.cif.'
_cod_original_cell_volume        1481.22(15)
_cod_database_code               7709038
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H20 N2 O2 Ce'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
The DMF was modeled as disordered over two positions related by a rotation about the metal carbonyl 
bond. The occupancy was originally linked to a free variable but refined to approximately 70:30 and 
was fixed at this for the rest of the refinement.
The hydrogens were located in a difference map but placed at calculated positions for the refinement.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O12 \\sim C13 \\sim N14 \\sim C14 \\sim C15: within 1.7A with sigma of 0.003
and sigma for terminal atoms of 0.006
3. Others
 Fixed Sof: C13(0.7) H13(0.7) N14(0.7) C14(0.7) H14A(0.7) H14B(0.7) H14C(0.7)
 C15(0.7) H15A(0.7) H15B(0.7) H15C(0.7) C13A(0.3) H13A(0.3) N14A(0.3) C14A(0.3)
 H14D(0.3) H14E(0.3) H14F(0.3) C15A(0.3) H15D(0.3) H15E(0.3) H15F(0.3)
4.a Free rotating group:
 O17(H17A,H17B)
4.b Rotating group:
 O16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C13(H13), C6(H6), C13A(H13A)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F), C15A(H15D,
 H15E,H15F)
;
_shelx_res_checksum              603
_shelx_hkl_checksum              35799
_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 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.687