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

data_7131850
_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         'C9 H17 B2 La, 0.667(C7 H8)'
_chemical_formula_sum            'C13.67 H22.33 B2 La'
_chemical_formula_weight         347.18
_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
_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.
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_cell_angle_alpha                85.128(12)
_cell_angle_beta                 86.013(11)
_cell_angle_gamma                75.462(13)
_cell_formula_units_Z            6
_cell_length_a                   8.2510(12)
_cell_length_b                   14.037(3)
_cell_length_c                   20.177(2)
_cell_measurement_reflns_used    38625
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.63
_cell_measurement_theta_min      2.44
_cell_volume                     2251.1(6)
_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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    SHELXT
_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 0.999
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_details
;
 526 frames, detector distance = 40 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_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25783
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.575
_diffrn_reflns_theta_min         2.439
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.821
_exptl_absorpt_correction_T_max  0.6752
_exptl_absorpt_correction_T_min  0.4471
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         11930
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10250
_reflns_number_total             11930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02717a2.cif
_cod_data_source_block           lmm127_test
_cod_database_code               7131850
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.602
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37C-C35C \\sim C35C-C41C
 with sigma of 0.02
 C41B-C35B \\sim C35B-C37B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35C \\sim C36C \\sim C37C \\sim C38C \\sim C39C \\sim C40C \\sim C41C: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C35B \\sim C36B \\sim C37B \\sim C38B \\sim C39B \\sim C40B \\sim C41B: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: C35A(0.6) H35A(0.6) H35B(0.6) H35C(0.6) C36A(0.6) C41A(0.6)
 H41A(0.6) C40A(0.6) H40A(0.6) C39A(0.6) H39A(0.6) C38A(0.6) H38A(0.6)
 C37A(0.6) H37A(0.6) C35B(0.26667) H35D(0.26667) H35E(0.26667) H35F(0.26667)
 C36B(0.26667) C41B(0.26667) H41B(0.26667) C40B(0.26667) H40B(0.26667)
 C39B(0.26667) H39B(0.26667) C38B(0.26667) H38B(0.26667) C37B(0.26667)
 H37B(0.26667) C35C(0.13333) H35G(0.13333) H35H(0.13333) H35I(0.13333)
 C36C(0.13333) C37C(0.13333) H37C(0.13333) C38C(0.13333) H38C(0.13333)
 C39C(0.13333) H39C(0.13333) C40C(0.13333) H40C(0.13333) C41C(0.13333)
 H41C(0.13333)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C41A(H41A), C40A(H40A), C39A(H39A), C38A(H38A),
 C37A(H37A), C41B(H41B), C40B(H40B), C39B(H39B), C38B(H38B), C37B(H37B),
 C37C(H37C), C38C(H38C), C39C(H39C), C40C(H40C), C41C(H41C)
5.b Fitted hexagon refined as free rotating group:
 C36A(C41A,C40A,C39A,C38A,C37A), C36B(C41B,C40B,C39B,C38B,C37B), C36C(C37C,
 C38C,C39C,C40C,C41C)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C35C(H35G,
 H35H,H35I)
;
_shelx_res_checksum              1305
_shelx_hkl_checksum              46728
_olex2_submission_special_instructions 'No special instructions were received'