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

data_7131848
_publ_section_title
;
 Mono-cyclononatetraenyl lanthanide complexes.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc02717a
_journal_year                    2023
_chemical_formula_moiety         'C13 H25 B2 Ce O'
_chemical_formula_sum            'C13 H25 B2 Ce O'
_chemical_formula_weight         359.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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
;
2023-06-05 deposited with the CCDC.	2023-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.499(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3380(6)
_cell_length_b                   8.7957(4)
_cell_length_c                   23.9487(15)
_cell_measurement_reflns_used    12441
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.47
_cell_volume                     1544.25(17)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.189.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.11.0 (STOE, 2022)
X-Area LANA 2.7.9.0 (STOE, 2022)
;
_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 2.3, Darmstadt 2023
;
_computing_structure_refinement  'SHELXL 2019/2 (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 0.999
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
 727 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_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12240
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.576
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.930
_exptl_absorpt_correction_T_max  0.8537
_exptl_absorpt_correction_T_min  0.4600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.514
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0514P)^2^+13.5898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3030
_reflns_number_total             3955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02717a2.cif
_cod_data_source_block           lmm186_amp2
_cod_database_code               7131848
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H2D-H2C \\sim H2C-H2B \\sim H2D-H2B
 with sigma of 0.02
 H2B-H2A \\sim H2A-H2C \\sim H2A-H2D
 with sigma of 0.02
 H1B-H1D \\sim H1D-H1A \\sim H1D-H1C
 with sigma of 0.02
 H1A-H1B \\sim H1B-H1C \\sim H1A-H1C
 with sigma of 0.02
 B1-H1A \\sim B1-H1C \\sim B1-H1B
 with sigma of 0.02
 B2-H2C \\sim B2-H2D \\sim B2-H2B
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C11(H11A,H11B), C12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C3(H3), C2(H2), C5(H5), C6(H6), C4(H4), C9(H9), C8(H8)
;
_shelx_res_checksum              62060
_shelx_hkl_checksum              13497
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '80.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '7.0 cm'
_stoe_detector_size_y            '8.4 cm'
_stoe_evaluation_integration_a   5.1
_stoe_evaluation_integration_b   -2.0
_stoe_evaluation_integration_ems 0.010
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 91.2
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 59.2
_stoe_evaluation_lana_max_2theta_desired 59.2
_stoe_evaluation_lana_mean_redundancy 3.1
_stoe_evaluation_lana_number_refls_after_or 12240
_stoe_evaluation_lana_number_refls_outliers 3333
_stoe_evaluation_lana_number_refls_total 15573
_stoe_evaluation_lana_number_refls_unique 3955
_stoe_evaluation_lana_number_refls_written 12240
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           7.1   13.3   19.5   25.7   31.9   38.1   44.3   50.5   56.7
<Resolution>    5.03   2.93   2.07   1.59   1.30   1.08   0.94   0.83   0.76
N(total)          48    422   1006   1790   2051   2631   3173   3094   1358
<Redundancy>     1.7    3.6    4.3    4.6    3.5    3.4    3.3    2.7    1.9
Complet. [%%]   100.0  100.0  100.0  100.0   99.8  100.0  100.0   99.1   63.9
<I/sigma>      102.8   53.7   39.7   24.2   18.5   11.2    7.4    4.4    2.9
R(int)         0.057  0.028  0.028  0.035  0.033  0.044  0.059  0.101  0.142
;
_stoe_measurement_identifier     LMM186_amp2
_stoe_measurement_max_exposure_per_frame '20.0 s'
_stoe_measurement_mean_exposure_per_frame '20.0 s'
_stoe_measurement_min_exposure_per_frame '20.0 s'
_stoe_measurement_total_exposure_time '4.0 h'
_stoe_measurement_total_frame_number 727
_stoe_measurement_total_run_number 10
_stoe_measurement_tube_power     '50.0 W'