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_7061206
_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 H42 La3 N6 O30, 2(H4 N), 2(H3 N), H2 N, 3.5(H O), 5(H2 O), [+ solvents]'
_chemical_formula_sum            'C31 H78.5 La3 N11 O42'
_chemical_formula_weight         1694.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                94.969(2)
_cell_angle_beta                 97.482(2)
_cell_angle_gamma                99.709(3)
_cell_formula_units_Z            4
_cell_length_a                   13.8336(5)
_cell_length_b                   17.2510(5)
_cell_length_c                   27.2896(7)
_cell_measurement_reflns_used    10234
_cell_measurement_temperature    143.00(10)
_cell_measurement_theta_max      28.0720
_cell_measurement_theta_min      3.2890
_cell_volume                     6325.1(3)
_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      143.00(10)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_details
;
  1 omega  -92.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309  -77.0000    0.0000 103

  2 omega  -40.00   36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   57.0000  -90.0000 76

  3 omega  -43.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   39.0000   90.0000 95

  4 omega  -30.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   57.0000  150.0000 79

  5 omega   25.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -99.0000 -180.0000 31

  6 omega  -42.00   -7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -57.0000 -150.0000 35

  7 omega    7.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   57.0000  -30.0000 49

  8 omega   62.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   57.0000  -60.0000 25

  9 omega    8.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -57.0000  -90.0000 25

 10 omega   68.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -178.0000 -150.0000 28

 11 omega   38.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809  -99.0000  -90.0000 28
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0078598000
_diffrn_orient_matrix_UB_12      -0.0355821000
_diffrn_orient_matrix_UB_13      -0.0126351000
_diffrn_orient_matrix_UB_21      -0.0482177000
_diffrn_orient_matrix_UB_22      -0.0188962000
_diffrn_orient_matrix_UB_23      0.0029733000
_diffrn_orient_matrix_UB_31      -0.0194780000
_diffrn_orient_matrix_UB_32      0.0117749000
_diffrn_orient_matrix_UB_33      -0.0229634000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            65391
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.111
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92486
_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    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             3394
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1565
_refine_ls_number_reflns         29117
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+9.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22177
_reflns_number_total             29117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05608e2.cif
_cod_data_source_block           exp_7500
_cod_depositor_comments
'Adding full bibliography for 7061206--7061210.cif.'
_cod_original_formula_sum        'C31 H78.50 La3 N11 O42'
_cod_database_code               7061206
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.679
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H7W of O7W, H4W of O4W, {H30A,H30B} of O30, {H59A,H59B}
  of O59, All N(H,H) groups, All N(H,H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  {H29A,H29B} of O29, {H58A,H58B} of O58, {H28A,H28B} of O28, H5W of O5W,
  H16W of O16W, H9W of O9W, H10W of O10W, {H6WA,H6WB} of O6W, {H8WA,H8WB} of
  O8W, {H2WA,H2WB} of O2W, {H12C,H12D} of O12W, {H11A,H11B} of O11W, {H1WA,
  H1WB} of O1W, {H17D,H17E} of O17W, {H13F,H13G} of O13W, {H15E,H15F} of O15W,
  {H3WA,H3WB} of O3W, H14W of O14W, {H60A,H60B} of O60
2. Restrained distances
 O30-H30A
 1 with sigma of 0.02
 O30-H30B
 1 with sigma of 0.02
 H10W-H58B
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O41) = Uanis(C40)
4.a Riding coordinates:
 N15(H15A,H15B,H15C), N15(H15D), N19(H19A,H19B,H19C), N19(H19D), N18(H18C,
 H18D), N18(H18E), N13(H13C,H13D), N13(H13E), N17(H17A,H17B), N17(H17C),
 N14(H14C), N14(H14D), N21(H21A,H21B), N21(H21C), N16(H16C), N16(H16D),
 N22(H22C,H22D,H22E), N22(H22F), N20(H20C,H20D,H20E), N20(H20F)
4.b Free rotating group:
 O7W(H7W), O5W(H5W), O16W(H16W), O9W(H9W), O10W(H10W), O6W(H6WA,H6WB),
 O8W(H8WA,H8WB), O2W(H2WA,H2WB), O12W(H12C,H12D), O11W(H11A,H11B), O1W(H1WA,
 H1WB), O17W(H17D,H17E), O13W(H13F,H13G), O4W(H4W), O15W(H15E,H15F), O3W(H3WA,
 H3WB), O14W(H14W)
4.c Rotating group:
 O29(H29A,H29B), O60(H60A,H60B), O28(H28A,H28B), O58(H58A,H58B)
4.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C44(H44A,H44B), C2(H2A,H2B), C24(H24A,H24B),
 C61(H61A,H61B), C59(H59C,H59D), C13(H13A,H13B), C20(H20A,H20B), C51(H51A,H51B),
  C22(H22A,H22B), C3(H3A,H3B), C23(H23A,H23B), C18(H18A,H18B), C47(H47A,H47B),
 C5(H5A,H5B), C41(H41A,H41B), C45(H45A,H45B), C26(H26A,H26B), C6(H6A,H6B),
 C16(H16A,H16B), C57(H57A,H57B), C30(H30C,H30D), C39(H39A,H39B), C43(H43A,H43B),
  C14(H14A,H14B), C55(H55A,H55B), C34(H34A,H34B), C12(H12A,H12B), C54(H54A,
 H54B), C53(H53A,H53B), C28(H28C,H28D), C49(H49A,H49B), C33(H33A,H33B),
 C35(H35A,H35B), C37(H37A,H37B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48209
_shelx_fab_checksum              12250
_olex2_submission_special_instructions 'No special instructions were received'