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_7710152
_publ_section_title
;
 Heavier Bis(m-terphenyl)element phosphaethynolates of Group 13
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00907B
_journal_year                    2022
_chemical_formula_moiety         'C56 H62 In N2 O P'
_chemical_formula_sum            'C56 H62 In N2 O P'
_chemical_formula_weight         924.86
_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             2022-01-18
_audit_creation_method
;
FinalCif V96 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-01-19 deposited with the CCDC.	2022-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.753(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2294(5)
_cell_length_b                   20.1471(12)
_cell_length_c                   22.3970(12)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.22
_cell_volume                     4978.1(5)
_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    'SHELXS (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91075
_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         25.999
_diffrn_reflns_theta_min         2.105
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0841 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8992.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.674
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0001P)^2^+25.8785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8776
_reflns_number_total             9791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00907b3.cif
_cod_data_source_block           janssenm201105_0m
_cod_database_code               7710152
_smtbx_masks_special_details
;
A solvent mask was calculated and 96 electrons were 
found in a volume of 450\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C7H8] per Asymmetric Unit 
which account for 100 electrons 
per unit cell.
;
_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. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O2')
Uanis(C13) = Uanis(C43)
3. Others
 Sof(P1')=Sof(O2')=Sof(In1')=1-FVAR(1)
 Sof(In1)=Sof(P1)=Sof(O1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C22(H22), C12(H12), C14(H14), C13(H13), C34(H34), C44(H44),
 C24(H24), C54(H54), C42(H42), C43(H43), C64(H64), C62(H62), C52(H52)
4.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C28(H28A,H28B,
 H28C), C37(H37A,H37B,H37C), C66(H66A,H66B,H66C), C58(H58A,H58B,H58C), C56(H56A,
 H56B,H56C), C27(H27A,H27B,H27C), C68(H68A,H68B,H68C), C6(H6A,H6B,H6C), C5(H5A,
 H5B,H5C), C67(H67A,H67B,H67C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), 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              72182
_shelx_hkl_checksum              28108
_shelx_fab_checksum              93935