CO reduction by calcium and ytterbium hydride complexes with a bulky monodentate carbazolyl ligand.
Hinz, Alexander; Winkler, Lucas; Sun, Xiaofei; Chemical communications (Cambridge, England) 60 (2024) 11291–11294; doi:10.1039/d4cc03714f

data_7133699
_publ_section_title
;
 CO reduction by calcium and ytterbium hydride complexes with a bulky
 monodentate carbazolyl ligand.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11291
_journal_page_last               11294
_journal_paper_doi               10.1039/d4cc03714f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C113.33 H150.67 N2 O3.33 Yb2'
_chemical_formula_sum            'C113.33 H150.67 N2 O3.33 Yb2'
_chemical_formula_weight         1940.43
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                66.923(4)
_cell_angle_beta                 84.961(4)
_cell_angle_gamma                85.933(4)
_cell_formula_units_Z            3
_cell_length_a                   14.3009(8)
_cell_length_b                   21.2924(11)
_cell_length_c                   27.1108(13)
_cell_measurement_reflns_used    47415
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.64
_cell_volume                     7559.3(7)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 1043 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1144
_diffrn_reflns_av_unetI/netI     0.1478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            101366
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.638
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    1.895
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.9590
_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            yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       plate
_exptl_crystal_F_000             3034
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.063
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2239
_refine_ls_number_reflns         29716
_refine_ls_number_restraints     2783
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1873
_refine_ls_R_factor_gt           0.0819
_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^)+(0.1263P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13919
_reflns_number_total             29716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03714f2.cif
_cod_data_source_block           XF492A
_cod_depositor_comments
'Adding full bibliography for 7133694--7133703.cif.'
_cod_database_code               7133699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              17484
_shelx_hkl_checksum              40223