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_7134388
_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 As1 Mo O2 P2'
_chemical_formula_sum            'C7 H5 As Mo O2 P2'
_chemical_formula_weight         353.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-01
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.8696(3)
_cell_length_b                   7.5409(2)
_cell_length_c                   24.3360(5)
_cell_measurement_reflns_used    10650
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      40.2480
_cell_measurement_theta_min      2.5040
_cell_volume                     1994.74(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -17.00  14.00   0.50    5.00    --  -10.90  98.00  27.00   62
  2  \w    -17.00   8.00   0.50    5.00    --  -10.90  25.00-124.00   50
  3  \w    -53.00 -28.00   0.50    5.00    --  -10.90 -25.00  71.00   50
  4  \w    -31.00  -6.00   0.50    5.00    --   11.05 -25.00  71.00   50
  5  \w     -1.00  32.00   0.50    5.00    --   11.05  25.00-124.00   66
  6  \w     20.00  56.00   0.50    5.00    --   11.05  57.00 -73.37   72
  7  \w    -38.00  20.00   0.50    5.00    --   11.05 -26.00   5.58  116
  8  \w    -38.00  17.00   0.50    5.00    --   11.05 -27.00 -46.27  110
  9  \w      8.00  43.00   0.50    5.00    --   11.05  83.00  10.37   70
 10  \w    -25.00  51.00   0.50    5.00    --   11.05   0.00  30.00  152
 11  \w     23.00  53.00   0.50    5.00    --   11.05  57.00  58.96   60
 12  \w      3.00  28.00   0.50    5.00    --   11.05  97.00  90.99   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      -0.0556634000
_diffrn_orient_matrix_UB_12      -0.0271571000
_diffrn_orient_matrix_UB_13      -0.0126637000
_diffrn_orient_matrix_UB_21      0.0267060000
_diffrn_orient_matrix_UB_22      0.0135309000
_diffrn_orient_matrix_UB_23      -0.0262605000
_diffrn_orient_matrix_UB_31      0.0210839000
_diffrn_orient_matrix_UB_32      -0.0890277000
_diffrn_orient_matrix_UB_33      -0.0001328000
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            39262
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.499
_diffrn_reflns_theta_min         2.513
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.888
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_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 intense yellow'
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0434P)^2^+2.6221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2562
_reflns_number_total             3047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01162k3.cif
_cod_data_source_block           lz703_fr1_mo_abs
_cod_depositor_comments
'Adding full bibliography for 7134388--7134391.cif.'
_cod_database_code               7134388
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C7 H5 O2 Mo P2 As'
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.641
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P3-Mo1
 2.6 with sigma of 0.02
 P4-P1 \\sim P5-P2 \\sim P6-P3
 with sigma of 0.02
 As1-P4 \\sim As3-P3 \\sim As2-P2
 with sigma of 0.02
 As1-P1 \\sim As3-P6 \\sim As2-P5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
As1 \\sim P1 \\sim P4 \\sim As3 \\sim P6 \\sim P3 \\sim As2 \\sim P2 \\sim P5:
within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
4. Others
 Fixed Sof: As1(0.68) P1(0.68) P4(0.68) As3(0.2) P6(0.2) P3(0.2) As2(0.12)
 P2(0.12) P5(0.12)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C2(H2), C5(H5), C3(H3)
;
_shelx_res_checksum              25844
_shelx_hkl_checksum              65833
_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 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.510