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

data_7131847
_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 La O'
_chemical_formula_sum            'C13 H25 B2 La O'
_chemical_formula_weight         357.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 93.184(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4353(5)
_cell_length_b                   7.2384(3)
_cell_length_c                   25.9862(15)
_cell_measurement_reflns_used    9115
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.50
_cell_volume                     1584.22(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details
;
 497 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  0.0243
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9000
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.410
_diffrn_reflns_theta_min         2.501
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  0.2861
_exptl_absorpt_correction_T_min  0.1824
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.635
_exptl_crystal_size_mid          0.545
_exptl_crystal_size_min          0.467
_refine_diff_density_max         0.777
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3242
_reflns_number_total             3948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02717a2.cif
_cod_data_source_block           lmm125_test
_cod_database_code               7131847
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C4(H4), C6(H6), C1(H1), C5(H5), C7(H7), C8(H8), C9(H9)
;
_shelx_res_checksum              33485
_shelx_hkl_checksum              95938
_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 0.011
_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 89.0
_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 59.1
_stoe_evaluation_lana_max_2theta_desired 59.1
_stoe_evaluation_lana_mean_redundancy 2.3
_stoe_evaluation_lana_number_refls_after_or 9000
_stoe_evaluation_lana_number_refls_outliers 1454
_stoe_evaluation_lana_number_refls_total 10454
_stoe_evaluation_lana_number_refls_unique 3948
_stoe_evaluation_lana_number_refls_written 9000
_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>    5.07   2.93   2.07   1.60   1.29   1.08   0.94   0.83   0.77
N(total)          36    315    676   1205   1492   1798   2136   1921    875
<Redundancy>     1.6    3.0    3.1    3.2    2.7    2.6    2.4    1.9    1.4
Complet. [%%]    83.3  100.0  100.0  100.0   99.3   99.8   99.7   97.9   56.6
<I/sigma>       99.7   63.2   47.7   32.8   23.5   14.7   10.5    7.4    5.7
R(int)         0.049  0.014  0.014  0.018  0.019  0.024  0.035  0.052  0.072
;
_stoe_measurement_identifier     LMM125_test
_stoe_measurement_max_exposure_per_frame '2.0 s'
_stoe_measurement_mean_exposure_per_frame '2.0 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '17 min'
_stoe_measurement_total_frame_number 497
_stoe_measurement_total_run_number 9
_stoe_measurement_tube_power     '50.0 W'