Highly water-soluble dimeric and trimeric lanthanide carbonates with ethylenediaminetetraacetates as precursors of catalysts for the oxidative coupling reaction of methane
Lin, Rong-Yan; Shi, Yan-Ru; Hou, Yu-Hui; Xia, Wen-Sheng; Weng, Wei-Zheng; Zhou, Zhao-Hui; New Journal of Chemistry 46 (2022) 3707–3715; doi:10.1039/D1NJ05608E

data_7061209
_publ_section_title
;
 Highly water-soluble dimeric and trimeric lanthanide carbonates with
 ethylenediaminetetraacetates as precursors of catalysts for the oxidative
 coupling reaction of methane
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3707
_journal_page_last               3715
_journal_paper_doi               10.1039/D1NJ05608E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety
'C31 H51.5 Ce3 K5 N6 O39, H2 O, 2.25[H2O], 0.5[H2O], 0.75[H2O]'
_chemical_formula_sum            'C31 H60.5 Ce3 K5 N6 O43.5'
_chemical_formula_weight         1829.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-10-13 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.641(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3813(7)
_cell_length_b                   15.2765(6)
_cell_length_c                   23.6607(9)
_cell_measurement_reflns_used    4150
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.2940
_cell_measurement_theta_min      3.4210
_cell_volume                     6428.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
  1 omega  -56.00   27.20   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1058   82.0000   14.0000 104

  2 omega  -18.00    9.20   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1058   57.0000  120.0000 34

  3 omega  -89.00  -34.60   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1058  -57.0000 -150.0000 68

  4 omega   13.00   88.20   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4339   57.0000 -180.0000 94

  5 omega  -11.00   31.40   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4339   82.0000  106.0000 53

  6 omega   53.00   90.60   0.8000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4339 -178.0000   60.0000 47
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0080700000
_diffrn_orient_matrix_UB_12      -0.0279647000
_diffrn_orient_matrix_UB_13      0.0247380000
_diffrn_orient_matrix_UB_21      -0.0191923000
_diffrn_orient_matrix_UB_22      0.0290159000
_diffrn_orient_matrix_UB_23      0.0146449000
_diffrn_orient_matrix_UB_31      -0.0340009000
_diffrn_orient_matrix_UB_32      -0.0230707000
_diffrn_orient_matrix_UB_33      -0.0115794000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36008
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.174
_diffrn_reflns_theta_min         2.945
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_description       block
_exptl_crystal_F_000             3622
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         14908
_refine_ls_number_restraints     529
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0199P)^2^+22.0285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11784
_reflns_number_total             14908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05608e2.cif
_cod_data_source_block           exp_2399
_cod_depositor_comments
'Adding full bibliography for 7061206--7061210.cif.'
_cod_original_formula_sum        'C31 H60.50 Ce3 K5 N6 O43.50'
_cod_database_code               7061209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.633
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H7WA,H7WB} of O7W, H1A of O1A, All C(H,H) groups
 At 1.5 times of:
  {H31C,H31D} of O31, {H1WA,H1WB} of O1W, {H6WA,H6WB} of O6W, {H9WA,H9WB} of
  O9W, {H3WA,H3WB} of O3W, H5W of O5W, {H28A,H28B} of O28, {H29A,H29B} of O29
2. Restrained distances
 O5W-H5W
 0.85 with sigma of 0.01
 H7WB-O30_$1
 1.9 with sigma of 0.02
 H7WB-O7W
 0.85 with sigma of 0.02
 O7W-H7WA
 0.85 with sigma of 0.02
 H7WA-O11
 1.9 with sigma of 0.02
 O15-H1WB
 1.9 with sigma of 0.02
 O1A-H1A
 0.85 with sigma of 0.02
 H1A-O27
 1.9 with sigma of 0.02
 K3-H5W
 3.614355 with sigma of 0.02
 O4W-H5W
 1.902699 with sigma of 0.02
 K5-H31C \\sim K5-H31D
 with sigma of 0.02
 Ce3-H29A \\sim Ce3-H29B
 with sigma of 0.02
 K3-H6WA \\sim K3-H6WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O22 \\sim O20 \\sim O14 \\sim O1 \\sim O23 \\sim O21 \\sim O2 \\sim O18 \\sim
O3 \\sim O12 \\sim O16 \\sim O4 \\sim O6 \\sim O26 \\sim O10 \\sim O8 \\sim O11
\\sim O24 \\sim O5 \\sim O30 \\sim O15 \\sim O7 \\sim O28 \\sim O13 \\sim O27
\\sim O29 \\sim O17 \\sim O19 \\sim O9 \\sim O25 \\sim O31 \\sim O2W \\sim O1W
\\sim O8W \\sim O6W \\sim O9W \\sim O3W \\sim O5W \\sim O7W \\sim O4W \\sim
O10W \\sim O1A: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
4. Others
 Fixed Sof: K6(0.5) O7W(0.75) H7WA(0.75) H7WB(0.75) O4W(0.25) O10W(0.5) O1A(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O7W(H7WA,H7WB), O1A(H1A)
5.b Free rotating group:
 O29(H29A,H29B), O31(H31C,H31D), O6W(H6WA,H6WB)
5.c Rotating group:
 O28(H28A,H28B), O9W(H9WA,H9WB), O3W(H3WA,H3WB)
5.d Ternary CH refined with riding coordinates:
 C10(H10A)
5.e Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C11(H11A,H11B), C13(H13A,H13B),
 C14(H14A,H14B), C16(H16A,H16B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C28(H28C,H28D), C29(H29C,
 H29D), C30(H30A,H30B), C31(H31A,H31B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46905
_shelx_fab_checksum              8603
_olex2_submission_special_instructions 'No special instructions were received'