Snapshots of sequential polyphosphide rearrangement upon metallatetrylene addition.
Sun, Xiaofei; Hinz, Alexander; Schulz, Stephan; Zimmermann, Lisa; Scheer, Manfred; Roesky, Peter W.; Chemical science 14 (2023) 4769–4776; doi:10.1039/d3sc00806a

data_1568875
_publ_section_title
;
 Snapshots of sequential polyphosphide rearrangement upon metallatetrylene
 addition.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              4769
_journal_page_last               4776
_journal_paper_doi               10.1039/d3sc00806a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '(C54 H79 As5 Cl Fe Ga Ge N4), 0.5(C6 D6)'
_chemical_formula_sum            'C57 H79 As5 Cl D3 Fe Ga Ge N4'
_chemical_formula_weight         1434.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-09 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.8546(6)
_cell_length_b                   16.4222(2)
_cell_length_c                   19.9888(4)
_cell_measurement_reflns_used    93305
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.46
_cell_volume                     12338.8(3)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area X-Red32 1.65.0.0 (STOE, 2018) 
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
 830 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88057
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.497
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    3.892
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.069
_refine_diff_density_max         3.018
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1430
_refine_ls_number_reflns         23772
_refine_ls_number_restraints     645
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0832P)^2^+57.2171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17428
_reflns_number_total             23772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00806a2.cif
_cod_data_source_block           xf470a_sq
_cod_depositor_comments
'Adding full bibliography for 1568870--1568876.cif.'
_cod_database_code               1568875
_shelx_shelxl_version_number     2019/2
_audit_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_audit_contact_letter
;
;
_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. Restrained distances
 C110-C111 \\sim C1A-C1C
 with sigma of 0.02
 C110-C109 \\sim C1A-C115
 with sigma of 0.02
 C114-C112 \\sim C1F-C1D
 with sigma of 0.04
 C111-C112 \\sim C1C-C1D
 with sigma of 0.02
 C111-C113 \\sim C1C-C1E
 with sigma of 0.04
 C114-C113 \\sim C1F-C1E
 with sigma of 0.02
 C109-C114 \\sim C115-C1F
 with sigma of 0.02
 C113-C112 \\sim C1E-C1D
 with sigma of 0.02
 C109-C113 \\sim C115-C1E
 with sigma of 0.04
 C110-C114 \\sim C1A-C1F
 with sigma of 0.04
 C110-C112 \\sim C1A-C1D
 with sigma of 0.04
 C111-C109 \\sim C1C-C115
 with sigma of 0.04
3. Rigid bond restraints
 C1, C1B, C2, C2B, C3, C3B, C4, C4B, C5, C5B, C6, C6B, C7, C7B, C8, C8B, C9,
 C9B, C10, C10B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C1B \\sim C2 \\sim C2B \\sim C3 \\sim C3B \\sim C4 \\sim C4B \\sim C5
\\sim C5B \\sim C6 \\sim C6B \\sim C7 \\sim C7B \\sim C8 \\sim C8B \\sim C9
\\sim C9B \\sim C10 \\sim C10B: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2.5A
C109 \\sim C114 \\sim C113 \\sim C112 \\sim C111 \\sim C110: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C1A \\sim C115 \\sim C1F \\sim C1E \\sim C1D \\sim C1C: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B} sigma for 1-2: 0.01, 1-3:
0.04
as in
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10}
6. Others
 Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=
 Sof(H6BC)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=
 Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
 Sof(C115)=Sof(D115)=Sof(C1F)=Sof(D1F)=Sof(C1E)=Sof(D1E)=Sof(C1D)=Sof(D1D)=
 Sof(C1C)=Sof(D1C)=Sof(C1A)=Sof(D1A)=1-FVAR(2)
 Sof(C110)=Sof(D110)=Sof(C109)=Sof(D109)=Sof(C114)=Sof(D114)=Sof(C113)=
 Sof(D113)=Sof(C112)=Sof(D112)=Sof(C111)=Sof(D111)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C32(H32), C35(H35), C49(H49), C52(H52), C86(H86), C89(H89), C103(H103),
 C106(H106)
7.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C28(H28), C29(H29),
 C30(H30), C40(H40), C45(H45), C46(H46), C47(H47), C71(H71), C72(H72), C73(H73),
  C74(H74), C75(H75), C82(H82), C83(H83), C84(H84), C94(H94), C99(H99),
 C100(H100), C101(H101), C110(D110), C109(D109), C114(D114), C113(D113),
 C112(D112), C111(D111), C115(D115), C1F(D1F), C1E(D1E), C1D(D1D), C1C(D1C),
 C1A(D1A)
7.c Fitted hexagon refined as free rotating group:
 C110(C109,C114,C113,C112,C111), C115(C1F,C1E,C1D,C1C,C1A)
7.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC),
 C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C87(H87A,
 H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C),
 C92(H92A,H92B,H92C), C96(H96A,H96B,H96C), C104(H10G,H10H,H10I), C105(H10J,H10K,
 H10L), C107(H10M,H10N,H10O), C108(H10P,H10Q,H10R)
;
_shelx_res_checksum              20407
_shelx_hkl_checksum              51266
_olex2_submission_special_instructions 'No special instructions were received'