Synthesis of heteropnictogen ligands via PI transfer
Zimmermann, Lisa; Land, Michael A.; Riesinger, Christoph; Macdonald, Charles L. B.; Scheer, Manfred; Chemical Communications 61 (2025) 6973–6976; doi:10.1039/D5CC01162K

data_7134389
_publ_section_title
;
 Synthesis of heteropnictogen ligands via PI transfer
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_page_first              6973
_journal_page_last               6976
_journal_paper_doi               10.1039/D5CC01162K
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C7 H5 Mo O2 P2.421 Sb0.579'
_chemical_formula_sum            'C7 H5 Mo O2 P2.42 Sb0.58'
_chemical_formula_weight         362.61
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-16
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.12950(10)
_cell_length_b                   11.38350(10)
_cell_length_c                   14.6754(2)
_cell_measurement_reflns_used    33288
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      40.8820
_cell_measurement_theta_min      2.2630
_cell_volume                     1017.48(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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      3.00  29.00   0.50    1.00    --  -10.90  35.00-172.16   52
  2  \w    -33.00  25.00   0.50    1.00    --   11.05 -19.00 -30.00  116
  3  \w    -26.00  28.00   0.50    1.00    --  -10.90  19.00  90.00  108
  4  \w    -30.00  13.00   0.50    1.00    --  -10.90   0.00 120.00   86
  5  \w    -17.00  17.00   0.50    1.00    --   11.05 -27.00 113.14   68
  6  \w     21.00  47.00   0.50    1.00    --   11.05  17.00  62.86   52
  7  \w     19.00  54.00   0.50    1.00    --   11.05  58.00 169.99   70
  8  \w    -23.00  45.00   0.50    1.00    --   11.05  19.00   0.00  136
  9  \w     33.00  59.00   0.50    1.00    --   11.05  19.00  30.00   52
 10  \w    -23.00   3.00   0.50    1.00    --   11.05  19.00  30.00   52
 11  \w    -22.00  10.00   0.50    1.00    --   11.05  17.00  62.86   64
 12  \w     27.00  55.00   0.50    1.00    --   11.05  51.00  -0.36   56
 13  \w     22.00  50.00   0.50    1.00    --   11.05  70.00-159.99   56
 14  \w     19.00  55.00   0.50    1.00    --   11.05  55.00-153.13   72
 15  \w    -14.00  12.00   0.50    1.00    --  -10.90 102.00 -84.97   52
 16  \w     -1.00  24.00   0.50    1.00    --   11.05  98.00-139.14   50
 17  \w     12.00  39.00   0.50    1.00    --   11.05  84.00-151.93   54
 18  \w      6.00  43.00   0.50    1.00    --   11.05  86.00-133.85   74
 19  \w     -8.00  24.00   0.50    1.00    --  -10.90  85.00 -27.10   64
 20  \w     -7.00  21.00   0.50    1.00    --  -10.90 100.00  78.91   56
 21  \w      8.00  33.00   0.50    1.00    --   11.05  83.00 111.20   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407341000
_diffrn_orient_matrix_UB_12      -0.0150027000
_diffrn_orient_matrix_UB_13      -0.0456428000
_diffrn_orient_matrix_UB_21      -0.1017430000
_diffrn_orient_matrix_UB_22      0.0269129000
_diffrn_orient_matrix_UB_23      0.0060077000
_diffrn_orient_matrix_UB_31      0.0391626000
_diffrn_orient_matrix_UB_32      0.0542109000
_diffrn_orient_matrix_UB_33      -0.0156840000
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46908
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.790
_diffrn_reflns_theta_min         2.270
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
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            'clear dark orange'
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0103P)^2^+0.6683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5845
_reflns_number_total             6515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01162k3.cif
_cod_data_source_block           lz704_fr1_mo2_abs
_cod_depositor_comments
'Adding full bibliography for 7134388--7134391.cif.'
_cod_database_code               7134389
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C7 H5 O2 Mo P2 Sb'
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.508
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Sb1 \\sim P1 \\sim P4 \\sim P6 \\sim P8 \\sim P2: within 2.5A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2.5A
3. Others
 Sof(P6)=Sof(P8)=Sof(P2)=1-FVAR(1)
 Sof(Sb1)=Sof(P1)=Sof(P4)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C2(H2), C5(H5), C3(H3)
;
_shelx_res_checksum              18282
_shelx_hkl_checksum              79468
_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 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.530