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_7133698
_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         'C102 H138 Ca2 N2 O3'
_chemical_formula_sum            'C102 H138 Ca2 N2 O3'
_chemical_formula_weight         1520.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 106.954(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5438(5)
_cell_length_b                   21.5053(4)
_cell_length_c                   26.0497(7)
_cell_measurement_reflns_used    29348
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      64.14
_cell_measurement_theta_min      2.91
_cell_volume                     9401.0(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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 2.0, Darmstadt 2021
;
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 EIGER4M
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      ' 927 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    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            31824
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         59.993
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           3.57
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_correction_T_min  0.6794
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10346
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0788P)^2^+0.6480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7308
_reflns_number_total             10346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03714f2.cif
_cod_data_source_block           AH1008A
_cod_depositor_comments
'Adding full bibliography for 7133694--7133703.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7133698
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              10981
_shelx_hkl_checksum              80326