Anilido-pyrazole ligand supported germylenes: synthesis, structure, and catalytic <i>N</i>-formylation of amines using CO<sub>2</sub>.
Barik, Jogendrananda; Rit, Arnab; Chemical communications (Cambridge, England) 62 (2026) 4131–4134; doi:10.1039/d5cc07160g

data_7135403
_publ_section_title
;
 Anilido-pyrazole ligand supported germylenes: synthesis, structure, and
 catalytic <i>N</i>-formylation of amines using CO<sub>2</sub>.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4131
_journal_page_last               4134
_journal_paper_doi               10.1039/d5cc07160g
_journal_volume                  62
_journal_year                    2026
_chemical_formula_sum            'C16 H14 Ge0.5 N3'
_chemical_formula_weight         284.6
_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
_atom_sites_solution_primary     'Intrinsic Phasing'
_audit_creation_method
;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-10-21 deposited with the CCDC.	2026-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.523(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5498(14)
_cell_length_b                   7.6080(7)
_cell_length_c                   18.5459(17)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    167(2)
_cell_measurement_theta_max      26.4067
_cell_measurement_theta_min      2.8946
_cell_measurement_wavelength     0.71073
_cell_volume                     2612.4(4)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      167(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega=   0.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega=   0.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 164.0; len= 184.0; end= 348.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg omega=   0.858 deg chi= -24.000 deg] 
measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 122.5; end= 127.5 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg phi= 204.000 deg chi= -44.500 deg] 
measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 122.5; end= 127.5 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg phi= 255.000 deg chi= -44.500 deg] 
measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 348.0; len= 184.0; end= 532.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg omega=   3.955 deg chi= -44.500 deg] 
measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   5.0; len= 122.5; end= 127.5 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   6.489 deg phi= 360.000 deg chi= -44.500 deg] 
measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   0.000 deg omega=   0.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26153
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         2.2
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.398
_diffrn_source_target            Mo
_diffrn_source_type              'INCOATEC I\mS 3.0'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+5.6799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2575
_reflns_number_total             2679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07160g2.cif
_cod_data_source_block           mo_Jogendra_CuPf6_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C16 H14 Ge0.50 N3'
_cod_database_code               7135403
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.916
_diffrn_measurement_bruker_total_exposure_time 10837.0
_diffrn_reflns_bruker_av_norm_i  1553.898
_diffrn_reflns_bruker_number_gt  32176
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              49158