Heavier Bis(m-terphenyl)element phosphaethynolates of Group 13
Duvinage, Daniel; Janssen, Marvin; Lork, Enno; Grützmacher, Hansjörg; Mebs, Stefan; Beckmann, Jens; Dalton Transactions  (2022) –; doi:10.1039/D2DT00907B

data_7710151
_publ_section_title
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 Heavier Bis(m-terphenyl)element phosphaethynolates of Group 13
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00907B
_journal_year                    2022
_chemical_formula_moiety         'C56 H62 In N2 O P Te'
_chemical_formula_sum            'C63 H70 In N2 O P Te'
_chemical_formula_weight         1144.60
_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     direct
_audit_creation_date             2022-01-17
_audit_creation_method
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FinalCif V96 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
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_audit_update_record
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2022-01-19 deposited with the CCDC.	2022-04-28 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 104.738(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4267(10)
_cell_length_b                   28.438(3)
_cell_length_c                   17.4895(14)
_cell_measurement_reflns_used    9738
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.79
_cell_measurement_theta_min      2.34
_cell_volume                     5496.3(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (G. Sheldrick)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            95732
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.263
_diffrn_reflns_theta_min         1.977
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0752 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.9106.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         21074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+2.9074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14438
_reflns_number_total             21074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00907b3.cif
_cod_data_source_block           janssenm210208_0m
_cod_database_code               7710151
_smtbx_masks_special_details
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A solvent mask was calculated and 190 electrons were 
found in a volume of 898\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C7H8] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
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_shelx_shelxl_version_number     2018/3
_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 Aromatic/amide H refined with riding coordinates:
 C32(H32), C42(H42), C43(H43), C44(H44), C34(H34), C22(H22), C62(H62),
 C24(H24), C14(H14), C52(H52), C12(H12), C64(H64), C13(H13), C54(H54)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C26(H26A,H26B,H26C), C5(H5A,H5B,
 H5C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C68(H68A,H68B,H68C), C8(H8A,
 H8B,H8C), C7(H7A,H7B,H7C), C37(H37A,H37B,H37C), C6(H6A,H6B,H6C), C27(H27A,H27B,
 H27C), C67(H67A,H67B,H67C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C57(H57A,
 H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 700'
_shelx_res_checksum              69117
_shelx_hkl_checksum              25252
_shelx_fab_checksum              34408