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_1568873
_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 N4 Si, 0.5(C6 H14)'
_chemical_formula_sum            'C57 H86 As5 Cl Fe Ga N4 Si'
_chemical_formula_weight         1391.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-06
_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                91.392(4)
_cell_angle_beta                 107.271(4)
_cell_angle_gamma                110.499(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5496(7)
_cell_length_b                   15.4580(8)
_cell_length_c                   16.9929(9)
_cell_measurement_reflns_used    55970
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.94
_cell_volume                     3150.6(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 2.5.3.0 (STOE, 2021)
X-Area X-Red 2.3.0.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 680 frames, detector distance = 40 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  0.0359
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47817
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.042
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    3.362
_exptl_absorpt_correction_T_max  0.7688
_exptl_absorpt_correction_T_min  0.3148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1418
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         13020
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0449P)^2^+0.4900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9861
_reflns_number_total             13020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00806a2.cif
_cod_data_source_block           xf464a
_cod_depositor_comments
'Adding full bibliography for 1568870--1568876.cif.'
_cod_database_code               1568873
_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
;
;
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.669
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C60-C59 \\sim C59-C58 \\sim C58-C57 \\sim C57-C56 \\sim C56-C55
 with sigma of 0.02
 C60-C58 \\sim C58-C56 \\sim C59-C57 \\sim C57-C55
 with sigma of 0.02
 C51-C52A \\sim C51-C52B
 with sigma of 0.02
 C52A-C53A \\sim C52B-C53B \\sim C52A-C54A \\sim C52B-C54B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C53A \\sim C52A \\sim C54A \\sim C51 \\sim C53B \\sim C54B \\sim C52B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C52B)=Sof(H52B)=Sof(C53B)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54B)=
 Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54A)=
 Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(1)
 Fixed Sof: C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) C57(0.5) H57A(0.5) H57B(0.5) C58(0.5) H58A(0.5) H58B(0.5) C59(0.5)
 H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5)
5.a Ternary CH refined with riding coordinates:
 C32(H32), C35(H35), C45(H45), C52A(H52A), C52B(H52B)
5.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
5.c 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), C48(H48), C49(H49), C50(H50)
5.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), 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), C39(H39A,
 H39B,H39C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C53A(H53A,H53B,H53C), C54A(H54A,H54B,H54C), C53B(H53D,H53E,H53F), C54B(H54D,
 H54E,H54F), C55(H55A,H55B,H55C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              24999
_shelx_hkl_checksum              96992
_olex2_submission_special_instructions 'No special instructions were received'