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

data_7131851
_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 La O5, C9 H9, C4 H8 O'
_chemical_formula_sum            'C33 H65 B2 La O6'
_chemical_formula_weight         718.38
_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
;
2023-06-05 deposited with the CCDC.	2023-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.126(3)
_cell_angle_beta                 93.934(3)
_cell_angle_gamma                94.032(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4435(3)
_cell_length_b                   9.0953(4)
_cell_length_c                   24.5660(9)
_cell_measurement_reflns_used    12867
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.49
_cell_volume                     1871.88(13)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_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      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
 714 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            87186
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.994
_diffrn_reflns_theta_min         2.251
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.8746
_exptl_absorpt_correction_T_min  0.5453
_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    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         87186
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0256P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                65071
_reflns_number_total             87186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02717a2.cif
_cod_data_source_block           lmm125__thf
_cod_database_code               7131851
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4999(4)
 0.5001(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C11-C12
 1.5 with sigma of 0.02
 C7A-C6A \\sim C7A-C8A \\sim C8A-C9A \\sim C9A-C1A \\sim C1A-C2A \\sim C3A-C2A
\\sim C4A-C3A \\sim C4A-C5A
 \\sim C5A-C6A
 with sigma of 0.01
 C3B-C4B \\sim C2B-C3B \\sim C2B-C1B \\sim C8B-C9B \\sim C1B-C9B \\sim C8B-C7B
\\sim C6B-C7B \\sim C6B-C5B
 \\sim C5B-C4B
 with sigma of 0.01
 C11-C12 \\sim C27-C28
 with sigma of 0.001
4. Rigid bond restraints
 C34, C35, C36, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C7A \\sim C8A \\sim C9A \\sim C1A \\sim C2A \\sim C4A \\sim C3A \\sim C5A \\sim
C6A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C4B \\sim C7B \\sim C5B \\sim C3B \\sim C6B \\sim C9B \\sim C1B \\sim C8B \\sim
C2B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
6. Others
 Fixed Sof: C2A(0.5) H2AA(0.5) C3A(0.5) H3A(0.5) C6A(0.5) H6A(0.5) C5A(0.5)
 H5A(0.5) C4A(0.5) H4A(0.5) C4B(0.5) H4B(0.5) C7B(0.5) H7B(0.5) C5B(0.5)
 H5B(0.5) C3B(0.5) H3B(0.5) C6B(0.5) H6B(0.5) C1A(0.5) H1AA(0.5) C9A(0.5)
 H9A(0.5) C8A(0.5) H8A(0.5) C7A(0.5) H7A(0.5) C9B(0.5) H9B(0.5) C1B(0.5)
 H1BA(0.5) C8B(0.5) H8B(0.5) C2B(0.5) H2BA(0.5) O6(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) C36(0.5) H36A(0.5) H36B(0.5) C35(0.5) H35A(0.5) H35B(0.5) O7(0.5)
 C37(0.5) H37A(0.5) H37B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C30(0.5) H30A(0.5) H30B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C20(H20A,H20B), C19(H19A,H19B), C18(H18A,H18B), C14(H14A,
 H14B), C26(H26A,H26B), C25(H25A,H25B), C28(H28A,H28B), C27(H27A,H27B),
 C23(H23A,H23B), C22(H22A,H22B), C17(H17A,H17B), C24(H24A,H24B), C13(H13A,H13B),
  C29(H29A,H29B), C10(H10A,H10B), C16(H16A,H16B), C15(H15A,H15B), C12(H12A,
 H12B), C11(H11A,H11B), C34(H34A,H34B), C36(H36A,H36B), C35(H35A,H35B),
 C37(H37A,H37B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B), C30(H30A,H30B)
7.b Aromatic/amide H refined with riding coordinates:
 C2A(H2AA), C3A(H3A), C6A(H6A), C5A(H5A), C4A(H4A), C4B(H4B), C7B(H7B),
 C5B(H5B), C3B(H3B), C6B(H6B), C1A(H1AA), C9A(H9A), C8A(H8A), C7A(H7A),
 C9B(H9B), C1B(H1BA), C8B(H8B), C2B(H2BA)
;
_shelx_res_checksum              99860
_shelx_hkl_checksum              91698
_olex2_submission_special_instructions 'No special instructions were received'