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_1568876
_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 Cl Fe Ga N4 P5 Si, 0.5(C6 D6)'
_chemical_formula_sum            'C57 H79 Cl D3 Fe Ga N4 P5 Si'
_chemical_formula_weight         1167.22
_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             2022-12-06
_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                90
_cell_angle_beta                 96.801(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.7246(8)
_cell_length_b                   16.1228(2)
_cell_length_c                   19.9295(4)
_cell_measurement_reflns_used    23499
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.77
_cell_volume                     12036.3(4)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      '215 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  0.0423
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            79223
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.774
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3921
_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    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1988
_refine_ls_number_reflns         23569
_refine_ls_number_restraints     4427
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0394P)^2^+26.4816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15099
_reflns_number_total             23569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00806a2.cif
_cod_data_source_block           xf458a
_cod_depositor_comments
'Adding full bibliography for 1568870--1568876.cif.'
_cod_original_cell_volume        12036.4(4)
_cod_original_formula_sum        'C57 H79 Cl Fe Ga N4 P5 Si D3'
_cod_database_code               1568876
_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   0.922
_shelx_estimated_absorpt_t_min   0.845
_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. Rigid bond restraints
 C1, C1B, C1C, C2, C2B, C2C, C3, C3B, C3C, C4, C4B, C4C, C5, C5B, C5C, C6, C6B,
  C6C, C7, C7B, C7C, C8, C8B, C8C, C9, C9B, C9C, C10, C10B, C10C
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 Si1C, Si2, N1C, N2C, N5, N6, C11, C11C, C12, C12C, C13, C13C, C14, C14C, C15,
 C15C, C16, C16C, C17, C17C, C18, C18C, C19, C19C, C20, C20C, C21, C21C, C22,
 C22C, C23, C23C, C24, C24C, C25, C25C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Fe1B, Fe1C, P1B, P1C, P2B, P2C, P3B, P3C, P4B, P4C, P5B, P5C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C26B, C27, C27B, C28, C28B, C29, C29B, C30, C30B, C31, C31B, C32, C32B,
 C33, C33B, C34, C34B, C35, C35B, C36, C36B, C37, C37B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C43B, C44, C44B, C45, C45B, C46, C46B, C47, C47B, C48, C48B, C49, C49B,
 C50, C50B, C51, C51B, C52, C52B, C53, C53B, C54, C54B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C1B \\sim C1C \\sim C2 \\sim C2B \\sim C2C \\sim C3 \\sim C3B \\sim
C3C \\sim C4 \\sim C4B \\sim C4C \\sim C5 \\sim C5B \\sim C5C \\sim C6 \\sim
C6B \\sim C6C \\sim C7 \\sim C7B \\sim C7C \\sim C8 \\sim C8B \\sim C8C \\sim
C9 \\sim C9B \\sim C9C \\sim C10 \\sim C10B \\sim C10C: within 2.5A with sigma
of 0.03 and sigma for terminal atoms of 0.06 within 2.5A
Si1C \\sim Si2 \\sim N1C \\sim N2C \\sim N5 \\sim N6 \\sim C11 \\sim C11C \\sim
C12 \\sim C12C \\sim C13 \\sim C13C \\sim C14 \\sim C14C \\sim C15 \\sim C15C
\\sim C16 \\sim C16C \\sim C17 \\sim C17C \\sim C18 \\sim C18C \\sim C19 \\sim
C19C \\sim C20 \\sim C20C \\sim C21 \\sim C21C \\sim C22 \\sim C22C \\sim C23
\\sim C23C \\sim C24 \\sim C24C \\sim C25 \\sim C25C: within 2.5A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2.5A
Fe1B \\sim Fe1C \\sim P1B \\sim P1C \\sim P2B \\sim P2C \\sim P3B \\sim P3C
\\sim P4B \\sim P4C \\sim P5B \\sim P5C: within 3.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.5A
C26 \\sim C26B \\sim C27 \\sim C27B \\sim C28 \\sim C28B \\sim C29 \\sim C29B
\\sim C30 \\sim C30B \\sim C31 \\sim C31B \\sim C32 \\sim C32B \\sim C33 \\sim
C33B \\sim C34 \\sim C34B \\sim C35 \\sim C35B \\sim C36 \\sim C36B \\sim C37
\\sim C37B: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2.5A
C43 \\sim C43B \\sim C44 \\sim C44B \\sim C45 \\sim C45B \\sim C46 \\sim C46B
\\sim C47 \\sim C47B \\sim C48 \\sim C48B \\sim C49 \\sim C49B \\sim C50 \\sim
C50B \\sim C51 \\sim C51B \\sim C52 \\sim C52B \\sim C53 \\sim C53B \\sim C54
\\sim C54B: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2.5A
C109 \\sim C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C209 \\sim
C210 \\sim C211 \\sim C212 \\sim C213 \\sim C214: within 2.5A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2.5A
4. Same fragment restrains
{Fe1B, P5B, P4B, P3B, P2B, P1B} sigma for 1-2: 0.01, 1-3: 0.04
{Fe1C, P5C, P4C, P3C, P2C, P1C} sigma for 1-2: 0.01, 1-3: 0.04
as in
{Fe2, P6, P7, P8, P9, P10}
{Si1C, N1C, N2C, C11C, C12C, C13C, C14C, C15C, C16C, C17C, C18C, C19C, C20C,
C21C, C22C, C23C, C24C, C25C} sigma for 1-2: 0.01, 1-3: 0.04
as in
{Si2, N5, N6, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23,
C24, C25}
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B} sigma for 1-2: 0.01, 1-3:
0.04
{C1C, C2C, C3C, C4C, C5C, C6C, C7C, C8C, C9C, C10C} sigma for 1-2: 0.01, 1-3:
0.04
as in
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10}
{C26B, C27B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, C35B, C36B, C37B} sigma
for 1-2: 0.01, 1-3: 0.04
as in
{C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37}
{C43B, C44B, C45B, C46B, C47B, C48B, C49B, C50B, C51B, C52B, C53B, C54B} sigma
for 1-2: 0.01, 1-3: 0.04
as in
{C43, C44, C45, C46, C47, C48, C49, C50, C51, C52, C53, C54}
5. Others
 1*[Sof(Fe2)+Sof(P6)+Sof(P7)+Sof(P8)+Sof(P9)+Sof(P10)]+1*[Sof(Fe1B)+Sof(P5B)+
 Sof(P4B)+Sof(P3B)+Sof(P2B)+Sof(P1B)]+1*[Sof(Fe1C)+Sof(P5C)+Sof(P4C)+Sof(P3C)+
 Sof(P2C)+Sof(P1C)]=1 with esd of 0
 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)]+1*[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*[Sof(C1C)+Sof(C2C)+Sof(C3C)+Sof(C4C)+Sof(C5C)+Sof(C6C)+Sof(H6CA)+
 Sof(H6CB)+Sof(H6CC)+Sof(C7C)+Sof(H7CA)+Sof(H7CB)+Sof(H7CC)+Sof(C8C)+Sof(H8CA)+
 Sof(H8CB)+Sof(H8CC)+Sof(C9C)+Sof(H9CA)+Sof(H9CB)+Sof(H9CC)+Sof(C10C)+Sof(H10G)+
 Sof(H10H)+Sof(H10I)]=1 with esd of 0
 Sof(Fe2)=Sof(P6)=Sof(P7)=Sof(P8)=Sof(P9)=Sof(P10)=FVAR(1)
 Sof(Fe1B)=Sof(P5B)=Sof(P4B)=Sof(P3B)=Sof(P2B)=Sof(P1B)=FVAR(2)
 Sof(Fe1C)=Sof(P5C)=Sof(P4C)=Sof(P3C)=Sof(P2C)=Sof(P1C)=FVAR(3)
 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(4)
 Sof(Si1C)=Sof(N1C)=Sof(N2C)=Sof(C11C)=Sof(C12C)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13C)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14C)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15C)=Sof(C16C)=Sof(C17C)=Sof(H17C)=Sof(C18C)=Sof(H18C)=
 Sof(C19C)=Sof(H19C)=Sof(C20C)=Sof(H20C)=Sof(C21C)=Sof(H21C)=Sof(C22C)=
 Sof(C23C)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24C)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C25C)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(5)
 Sof(Si2)=Sof(N5)=Sof(N6)=Sof(C11)=Sof(C12)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(C23)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=FVAR(5)
 Sof(C26B)=Sof(C27B)=Sof(C28B)=Sof(H28B)=Sof(C29B)=Sof(H29B)=Sof(C30B)=
 Sof(H30B)=Sof(C31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35B)=
 Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37B)=Sof(H37D)=Sof(H37E)=
 Sof(H37F)=1-FVAR(6)
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=
 Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=
 Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(6)
 Sof(C43B)=Sof(C44B)=Sof(C45B)=Sof(H45B)=Sof(C46B)=Sof(H46B)=Sof(C47B)=
 Sof(H47B)=Sof(C48B)=Sof(C49B)=Sof(H49B)=Sof(C50B)=Sof(H50D)=Sof(H50E)=
 Sof(H50F)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=Sof(H52B)=
 Sof(C53B)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54B)=Sof(H54D)=Sof(H54E)=
 Sof(H54F)=1-FVAR(7)
 Sof(C43)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(7)
 Sof(C209)=Sof(H209)=Sof(C210)=Sof(H210)=Sof(C211)=Sof(H211)=Sof(C212)=
 Sof(H212)=Sof(C213)=Sof(H213)=Sof(C214)=Sof(H214)=1-FVAR(8)
 Sof(C109)=Sof(H109)=Sof(C110)=Sof(H110)=Sof(C111)=Sof(H111)=Sof(C112)=
 Sof(H112)=Sof(C113)=Sof(H113)=Sof(C114)=Sof(H114)=FVAR(8)
 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)=FVAR(9)
 Sof(C1C)=Sof(C2C)=Sof(C3C)=Sof(C4C)=Sof(C5C)=Sof(C6C)=Sof(H6CA)=Sof(H6CB)=
 Sof(H6CC)=Sof(C7C)=Sof(H7CA)=Sof(H7CB)=Sof(H7CC)=Sof(C8C)=Sof(H8CA)=Sof(H8CB)=
 Sof(H8CC)=Sof(C9C)=Sof(H9CA)=Sof(H9CB)=Sof(H9CC)=Sof(C10C)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=FVAR(10)
6.a Ternary CH refined with riding coordinates:
 C86(H86), C89(H89), C103(H103), C106(H106), C32(H32), C35(H35), C32B(H32B),
 C35B(H35B), C49(H49), C52(H52), C49B(H49B), C52B(H52B)
6.b Me refined with riding coordinates:
 C12C(H12A,H12B,H12C), C13C(H13A,H13B,H13C), C14C(H14A,H14B,H14C), C23C(H23A,
 H23B,H23C), C24C(H24A,H24B,H24C), C25C(H25A,H25B,H25C)
6.c Aromatic/amide H refined with riding coordinates:
 C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C82(H82), C83(H83),
 C84(H84), C94(H94), C99(H99), C100(H100), C101(H101), C17C(H17C), C18C(H18C),
 C19C(H19C), C20C(H20C), C21C(H21C), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C28(H28), C29(H29), C30(H30), C28B(H28B), C29B(H29B), C30B(H30B),
 C40(H40), C45(H45), C46(H46), C47(H47), C45B(H45B), C46B(H46B), C47B(H47B),
 C109(H109), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114),
 C209(H209), C210(H210), C211(H211), C212(H212), C213(H213), C214(H214)
6.d Fitted pentagon refined as free rotating group:
 C1(C2,C3,C4,C5), C1B(C2B,C3B,C4B,C5B), C1C(C2C,C3C,C4C,C5C)
6.e Fitted hexagon refined as free rotating group:
 C43B(C44B,C45B,C46B,C47B,C48B), C109(C110,C111,C112,C113,C114), C209(C210,
 C211,C212,C213,C214)
6.f Idealised Me refined as rotating group:
 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(H10J,H10K,H10L),
 C105(H10M,H10N,H10O), C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C12(H12D,
 H12E,H12F), C13(H13D,H13E,H13F), C14(H14D,H14E,H14F), C23(H23D,H23E,H23F),
 C24(H24D,H24E,H24F), C25(H25D,H25E,H25F), 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), C6C(H6CA,H6CB,H6CC), C7C(H7CA,H7CB,H7CC), C8C(H8CA,H8CB,H8CC), C9C(H9CA,
 H9CB,H9CC), C10C(H10G,H10H,H10I), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C33B(H33D,H33E,H33F), C34B(H34D,H34E,
 H34F), C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F), C38(H38A,H38B,H38C),
 C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C50B(H50D,H50E,H50F), C51B(H51D,H51E,H51F),
 C53B(H53D,H53E,H53F), C54B(H54D,H54E,H54F)
;
_shelx_res_checksum              6504
_shelx_hkl_checksum              83093
_olex2_submission_special_instructions 'No special instructions were received'