Mono-cyclononatetraenyl lanthanide complexes.
Münzfeld, Luca; Hauser, Adrian; Gamer, Michael T.; Roesky, Peter W.; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc02717a

data_7131849
_publ_section_title
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 Mono-cyclononatetraenyl lanthanide complexes.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc02717a
_journal_year                    2023
_chemical_formula_moiety         'C20 H48 B2 Ce O5, C4 H8 O, C9 H9'
_chemical_formula_sum            'C33 H65 B2 Ce O6'
_chemical_formula_weight         719.59
_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             2023-05-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2023-06-05 deposited with the CCDC.	2023-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.106(4)
_cell_angle_beta                 93.801(4)
_cell_angle_gamma                94.191(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3963(4)
_cell_length_b                   9.0379(4)
_cell_length_c                   24.4820(11)
_cell_measurement_reflns_used    16727
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.27
_cell_volume                     1843.31(15)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)'
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details
;
 1296 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48567
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.731
_diffrn_reflns_theta_min         2.266
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.4420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.193
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         48567
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0736P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33495
_reflns_number_total             48567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02717a2.cif
_cod_data_source_block           lmm186_thf
_cod_database_code               7131849
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.630
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.4165(8)
 0.5835(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 Ce-H2D \\sim Ce-H2C \\sim Ce-H2B
 with sigma of 0.01
 B1-H1B \\sim B1-H1C \\sim B1-H1D
 with sigma of 0.01
 C9A-C1A \\sim C9A-C8A \\sim C8A-C7A \\sim C7A-C6A \\sim C6A-C5A \\sim C5A-C4A
\\sim C4A-C3A \\sim C3A-C2A
 \\sim C2A-C1A
 with sigma of 0.02
 Ce-H1B \\sim Ce-H1C \\sim Ce-H1D
 with sigma of 0.01
 H1B-H1D \\sim H1D-H1C \\sim H1B-H1C
 with sigma of 0.02
 B2-H2D \\sim B2-H2C \\sim B2-H2B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C1A \\sim
C2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C25 \\sim C24B \\sim C23B \\sim C22 \\sim O4: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
C23A \\sim C24A \\sim C25 \\sim O4 \\sim C22: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C1B \\sim C8B \\sim C9B \\sim C7B \\sim C6B \\sim C5B \\sim C4B \\sim C3B \\sim
C2B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Fixed Sof: H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) C23A(0.5) H23A(0.5) H23B(0.5) C30(0.5) H30A(0.5) H30B(0.5) C6B(0.5)
 H6B(0.5) C4B(0.5) H4B(0.5) O6(0.5) C5B(0.5) H5B(0.5) C24B(0.5) H24A(0.5)
 H24B(0.5) C7B(0.5) H7B(0.5) C8B(0.5) H8B(0.5) C5A(0.5) H5A(0.5) C3A(0.5)
 H3A(0.5) C4A(0.5) H4A(0.5) O7(0.5) C34(0.5) H34A(0.5) H34B(0.5) C37(0.5)
 H37A(0.5) H37B(0.5) C36(0.5) H36A(0.5) H36B(0.5) C35(0.5) H35A(0.5) H35B(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C7A(0.5) H7A(0.5)
 C2A(0.5) H2AA(0.5) C1B(0.5) H1BA(0.5) C9B(0.5) H9B(0.5) C2B(0.5) H2BA(0.5)
 C3B(0.5) H3B(0.5) C6A(0.5) H6A(0.5) C9A(0.5) H9A(0.5) C8A(0.5) H8A(0.5)
 C1A(0.5) H1AA(0.5) H25C(0.5) H25D(0.5) H25A(0.5) H25B(0.5) C24A(0.5) H24C(0.5)
 H24D(0.5) C23B(0.5) H23C(0.5) H23D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C26(H26A,H26B), C10(H10A,H10B), C14(H14A,
 H14B), C11(H11A,H11B), C20(H20A,H20B), C18(H18A,H18B), C29(H29A,H29B),
 C19(H19A,H19B), C22(H22A,H22B), C22(H22C,H22D), C16(H16A,H16B), C15(H15A,H15B),
  C17(H17A,H17B), C27(H27A,H27B), C21(H21A,H21B), C31(H31A,H31B), C23A(H23A,
 H23B), C30(H30A,H30B), C28(H28A,H28B), C24B(H24A,H24B), C34(H34A,H34B),
 C37(H37A,H37B), C36(H36A,H36B), C35(H35A,H35B), C32(H32A,H32B), C33(H33A,H33B),
  C25(H25C,H25D), C25(H25A,H25B), C24A(H24C,H24D), C23B(H23C,H23D)
6.b Aromatic/amide H refined with riding coordinates:
 C6B(H6B), C4B(H4B), C5B(H5B), C7B(H7B), C8B(H8B), C5A(H5A), C3A(H3A),
 C4A(H4A), C7A(H7A), C2A(H2AA), C1B(H1BA), C9B(H9B), C2B(H2BA), C3B(H3B),
 C6A(H6A), C9A(H9A), C8A(H8A), C1A(H1AA)
;
_shelx_res_checksum              82241
_shelx_hkl_checksum              90681
_olex2_submission_special_instructions 'No special instructions were received'