Vinyl-pyrazole as a biomimetic acetaldehyde surrogate.
Steiner, Lorenz; Ćorović, Miljan Z; Dupé, Antoine; Mösch-Zanetti, Nadia C; Chemical communications (Cambridge, England) 60 (2024) 6873–6876; doi:10.1039/d4cc01305k

data_7133130
_publ_section_title
;
 Vinyl-pyrazole as a biomimetic acetaldehyde surrogate.
;
_journal_issue                   54
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6873
_journal_page_last               6876
_journal_paper_doi               10.1039/d4cc01305k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C10 H11 Br2 N3 O3 W, C H Cl3'
_chemical_formula_sum            'C11 H12 Br2 Cl3 N3 O3 W'
_chemical_formula_weight         684.26
_chemical_name_systematic
'fac-tricarbonyl-dibromo-(1-(1-iminoethyl)-3,5-dimethylpyrazole-N,N')-tungsten(II) chloroform solvate'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-13
_audit_creation_method
;
Olex2 1.5-ac6-019
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6920)
;
_audit_update_record
;
2024-05-13 deposited with the CCDC.	2024-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                63.402(2)
_cell_angle_beta                 75.4980(10)
_cell_angle_gamma                79.6940(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2942(2)
_cell_length_b                   10.3885(2)
_cell_length_c                   11.1039(2)
_cell_measurement_reflns_used    22411
_cell_measurement_temperature    99.97(18)
_cell_measurement_theta_max      33.2630
_cell_measurement_theta_min      2.1960
_cell_volume                     925.34(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.92a 64-bit (release 05-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-019 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-019 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00   5.00   0.50    0.50    --   13.37 -19.00 120.00  148
  2  \w    -69.00   5.00   0.50    0.50    --   13.37 -19.00  30.00  148
  3  \w    -69.00   5.00   0.50    0.50    --   13.37 -19.00 -90.00  148
  4  \w    -69.00   1.00   0.50    0.50    --   13.37 -19.00 -30.00  140
  5  \w     42.00  90.00   0.50    0.50    --   13.37 178.00-180.00   96
  6  \w    -69.00   5.00   0.50    0.50    --   13.37 -19.00-180.00  148
  7  \w    -23.00  28.00   0.50    0.50    --  -15.09 -99.00 -60.00  102
  8  \w    -23.00  28.00   0.50    0.50    --  -15.09 -99.00-180.00  102
  9  \w    -93.00   9.00   0.50    0.50    --  -15.09 -57.00  90.00  204
 10  \w    -93.00   9.00   0.50    0.50    --  -15.09 -57.00  90.00  204
 11  \w    -23.00  57.00   0.50    0.50    --   13.37 -99.00  90.00  160
 12  \w     24.00  86.00   0.50    0.50    --   13.37-146.00  20.00  124
 13  \w     13.00  74.00   0.50    0.50    --   13.37-126.00-172.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489675000
_diffrn_orient_matrix_UB_12      0.0193641000
_diffrn_orient_matrix_UB_13      0.0505531000
_diffrn_orient_matrix_UB_21      0.0203089000
_diffrn_orient_matrix_UB_22      -0.0671001000
_diffrn_orient_matrix_UB_23      0.0521553000
_diffrn_orient_matrix_UB_31      0.0586576000
_diffrn_orient_matrix_UB_32      0.0314335000
_diffrn_orient_matrix_UB_33      0.0051436000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28243
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.270
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.007
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.107a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.456
_exptl_crystal_description       plate
_exptl_crystal_F_000             636
_exptl_crystal_recrystallization_method 'recrystallized in chloroform'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0136P)^2^+0.8592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5172
_reflns_number_total             5632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01305k2.cif
_cod_data_source_block           ad08
_cod_depositor_comments
'Adding full bibliography for 7133129--7133132.cif.'
_cod_database_code               7133130
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C11 H12 N3 O3 Cl3 Br2 W1 '
_chemical_oxdiff_usercomment     LST370
_shelx_estimated_absorpt_t_max   0.377
_shelx_estimated_absorpt_t_min   0.137
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6)
2.c Idealised Me refined as rotating group:
 C4(H41,H42,H43), C8(H81,H82,H83), C9(H91,H92,H93)
;
_shelx_res_checksum              9395
_shelx_hkl_checksum              43249
_olex2_date_sample_data_collection 2024-01-11
_olex2_date_sample_submission    2024-01-09
_olex2_exptl_crystal_mounting_method 'mounted on a glass fiber'
_olex2_submission_original_sample_id LST370
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.759