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_7133702
_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         'C54 H82 Ca N2 Si2'
_chemical_formula_sum            'C54 H82 Ca N2 Si2'
_chemical_formula_weight         855.47
_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   geom
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_audit_update_record
;
2022-01-29 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   16.2635(10)
_cell_length_c                   20.1945(10)
_cell_measurement_reflns_used    29127
_cell_measurement_temperature    200(2)
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_cell_volume                     5417.6(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
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;
X-Area Integrate 1.73.0.0 (STOE, 2018)
X-Area LANA 1.72.3.0 (STOE, 2018)
;
_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 1.82, Darmstadt 2018
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
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_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 154 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36337
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
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_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
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_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
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_exptl_crystal_description       block
_exptl_crystal_F_000             1872
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_exptl_crystal_size_mid          0.350
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0705P)^2^+1.2183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10093
_reflns_number_total             14389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03714f2.cif
_cod_data_source_block           AH982F
_cod_depositor_comments
'Adding full bibliography for 7133694--7133703.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7133702
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              71635
_shelx_hkl_checksum              82064