Photochemical formation and reversible base-induced cleavage of a phosphagallene.
Taeufer, T.; Dankert, F.; Michalik, D.; Pospech, J.; Bresien, J.; Hering-Junghans, C; Chemical science 14 (2023) 3018–3023; doi:10.1039/d2sc06292e

data_1568440
_publ_section_title
;
 Photochemical formation and reversible base-induced cleavage of a
 phosphagallene.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              3018
_journal_page_last               3023
_journal_paper_doi               10.1039/d2sc06292e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C46 H64 Ga P'
_chemical_formula_sum            'C46 H64 Ga P'
_chemical_formula_weight         717.66
_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             2022-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-11-01 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                80.8620(10)
_cell_angle_beta                 81.8580(10)
_cell_angle_gamma                65.9260(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6093(2)
_cell_length_b                   12.7651(2)
_cell_length_c                   20.7583(3)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      66.74
_cell_measurement_theta_min      4.17
_cell_volume                     2524.94(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32338
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.745
_diffrn_reflns_theta_max         66.745
_diffrn_reflns_theta_min         3.816
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'APEX2, SADABS was used for absorption correction.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.944
_exptl_crystal_description       plate
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8929
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0619P)^2^+1.2453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8147
_reflns_number_total             8929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06292e3.cif
_cod_data_source_block           ax2276_cu_TipTerPGaCpStar_Cmpd1b
_cod_depositor_comments
'Adding full bibliography for 1568439--1568441.cif.'
_cod_original_cell_volume        2524.95(7)
_cod_database_code               1568440
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.736
_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
 C29A-C28A = C30A-C28A = C29-C28 = C28-C30
 1.52 with sigma of 0.01
 C29A-C28A = C29-C28 = C28-C30 = C30A-C28A
 1.52 with sigma of 0.01
 C29A-C28A = C29-C28 = C30A-C28A = C28-C30
 1.52 with sigma of 0.001
 C35A-C34A = C36-C34
 1.52 with sigma of 0.001
 C31A-C32A
 1.52 with sigma of 0.002
 C31-C33 = C32-C31
 1.52 with sigma of 0.002
 C27-C34 \\sim C34A-C27A
 with sigma of 0.01
 C28-C23 \\sim C28A-C23
 with sigma of 0.01
 C25A-C31A \\sim C31-C25
 with sigma of 0.01
3. Restrained planarity
 C28A, C31A, C34A, C22, C27A, C26A, C25A, C24A, C23
 with sigma of 0.01
 C23, C24, C25, C27, C22, C26
 with sigma of 0.1
 C23, C24, C25, C26, C27, C22
 with sigma of 0.001
 C28, C23, C24, C25, C26, C27, C22, C31
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C27 \\sim C24 \\sim C24A \\sim C25A \\sim C25 \\sim C26 \\sim C26A \\sim C23
\\sim C22: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C27A \\sim C25A
\\sim C24A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 2A
Uanis(C25A) = Uanis(C25)
Uanis(C23) = Uanis(C28) = Uanis(C28A)
5. Rigid body (RIGU) restrains
 C22, C23, C24, C24A, C25, C25A, C26, C26A, C27, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C27A)=Sof(C26A)=Sof(H26A)=Sof(C25A)=Sof(C24A)=Sof(H24A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C33A)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C36A)=
 Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C34A)=Sof(H34A)=Sof(C31A)=
 Sof(H31A)=1-FVAR(1)
 Sof(C27)=Sof(C26)=Sof(H26)=Sof(C25)=Sof(C24)=Sof(H24)=Sof(C34)=Sof(H34)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C31)=Sof(H31)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29D)=Sof(H29E)=Sof(H29F)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C19(H19), C13(H13), C16(H16), C28A(H28A), C34(H34), C31(H31), C34A(H34A),
 C31A(H31A), C28(H28)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C26(H26), C24(H24), C26A(H26A), C24A(H24A), C11(H11), C5(H5), C3(H3),
 C4(H4)
7.c Fitted hexagon refined as free rotating group:
 C22(C27,C26,C25,C24,C23)
7.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C44(H44A,H44B,
 H44C), C18(H18A,H18B,H18C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C20(H20A,
 H20B,H20C), C17(H17A,H17B,H17C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C30(H30A,H30B,H30C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C33(H33A,H33B,
 H33C), C29A(H29A,H29B,H29C), C33A(H33D,H33E,H33F), C32A(H32A,H32B,H32C),
 C32(H32D,H32E,H32F), C36A(H36D,H36E,H36F), C35A(H35D,H35E,H35F), C30A(H30D,
 H30E,H30F), C29(H29D,H29E,H29F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68372
_shelx_hkl_checksum              39306
_shelx_fab_checksum              11497
_olex2_submission_special_instructions 'No special instructions were received'