Modulating the reactivity of phosphanylidenephosphoranes towards water with Lewis acids
Dankert, Fabian; Fischer, Malte; Hering-Junghans, Christian; Dalton Transactions  (2022) –; doi:10.1039/D2DT01575G

data_7710530
_publ_section_title
;
 Modulating the reactivity of phosphanylidenephosphoranes towards water
 with Lewis acids
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01575G
_journal_year                    2022
_chemical_formula_moiety         '4(C54 H68 Cl2 Ga P4), 4(Cl4 Ga)'
_chemical_formula_sum            'C54 H68 Cl6 Ga2 P4'
_chemical_formula_weight         1193.10
_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             2022-03-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-04-14 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                109.535(7)
_cell_angle_beta                 97.030(7)
_cell_angle_gamma                90.092(7)
_cell_formula_units_Z            4
_cell_length_a                   12.9253(12)
_cell_length_b                   21.2504(19)
_cell_length_c                   24.984(2)
_cell_measurement_reflns_used    13037
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      1.53
_cell_volume                     6412.0(10)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_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 1.3 (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 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 329 frames, detector distance = 110 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.1210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            71835
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.548
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.500
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.4878
_exptl_absorpt_correction_T_min  0.4283
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1147
_refine_ls_number_reflns         23897
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0953P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1839
_reflns_d_resolution_high        0.756
_reflns_d_resolution_low         13.157
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              28
_reflns_limit_k_min              -28
_reflns_limit_l_max              32
_reflns_limit_l_min              -32
_reflns_number_gt                11059
_reflns_number_total             23897
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt01575g2.cif
_cod_data_source_block           ks1572_cmpd_9MesTer
_cod_database_code               7710530
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.792
_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
C83 \\sim C82 \\sim C81 \\sim C89 \\sim C87 \\sim C88 \\sim C92 \\sim C93 \\sim
C27 \\sim C28 \\sim C29 \\sim C3 \\sim C4 \\sim C5 \\sim C23 \\sim C18 \\sim
C19 \\sim C20 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C83) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C83, C82, C81, C89, C87, C88, C92, C93, C27, C28, C29, C3, C4, C5, C23, C18,
 C19, C20, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 2
4.a Me refined with riding coordinates:
 C76(H76A,H76B,H76C), C38(H38A,H38B,H38C), C15(H15A,H15B,H15C), C48(H48A,H48B,
 H48C), C68(H68A,H68B,H68C), C92(H92A,H92B,H92C)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C18(H18), C35(H35), C87(H87), C89(H89), C5(H5), C4(H4), C3(H3),
 C11(H11), C96(H96), C98(H98), C65(H65), C57(H57), C58(H58), C59(H59), C72(H72),
  C9(H9), C63(H63), C33(H33), C83(H83), C82(H82), C81(H81), C44(H44), C74(H74),
 C42(H42), C29(H29), C27(H27), C28(H28)
4.c Fitted hexagon refined as free rotating group:
 C16(C21,C20,C19,C18,C17), C85(C86,C87,C88,C89,C90), C1(C6,C5,C4,C3,C2),
 C97(C96,C95,C94,C99,C98), C55(C56,C57,C58,C59,C60), C79(C84,C83,C82,C81,C80)
4.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C108(H10A,H10B,
 H10C), C104(H10D,H10E,H10F), C106(H10G,H10H,H10I), C22(H22A,H22B,H22C),
 C67(H67A,H67B,H67C), C52(H52A,H52B,H52C), C50(H50A,H50B,H50C), C103(H10J,H10K,
 H10L), C107(H10M,H10N,H10O), C105(H10P,H10Q,H10R), C53(H53A,H53B,H53C),
 C77(H77A,H77B,H77C), C91(H91A,H91B,H91C), C101(H10S,H10T,H10U), C69(H69A,H69B,
 H69C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C37(H37A,H37B,H37C), C13(H13A,
 H13B,H13C), C102(H10V,H10W,H10X), C75(H75A,H75B,H75C), C14(H14A,H14B,H14C),
 C24(H24A,H24B,H24C), C100(H10Y,H,HA), C47(H47A,H47B,H47C), C23(H23A,H23B,H23C),
  C93(H93A,H93B,H93C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34772
_shelx_hkl_checksum              69543
_shelx_fab_checksum              48643
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '110.0 mm'
_stoe_detector_pixelsize_x       '0.150 mm'
_stoe_detector_pixelsize_y       '0.150 mm'
_stoe_detector_size_x            '34.0 cm'
_stoe_detector_size_y            '34.0 cm'
_stoe_evaluation_integration_a   12.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 98.7
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 56.1
_stoe_evaluation_lana_max_2theta_desired 56.1
_stoe_evaluation_lana_mean_redundancy 3.0
_stoe_evaluation_lana_number_refls_after_or 92211
_stoe_evaluation_lana_number_refls_outliers 9446
_stoe_evaluation_lana_number_refls_total 101657
_stoe_evaluation_lana_number_refls_unique 30677
_stoe_evaluation_lana_number_refls_written 92211
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta           5.6   11.6   17.6   23.6   29.6   35.6   41.6   47.6   53.6
<Resolution>    6.14   3.37   2.28   1.72   1.38   1.16   1.00   0.88   0.79
N(total)         447   1723   3924   6750  10274  14155  18717  22823  22844
<Redundancy>     2.7    2.8    2.9    2.9    3.0    3.0    3.0    3.1    3.0
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   94.7
<I/sigma>      102.7   58.3   22.3   16.4    6.3    3.4    1.7    0.7    0.2
R(int)         0.015  0.019  0.025  0.029  0.062  0.105  0.187  0.378  0.614
;
_stoe_measurement_identifier     ks1572
_stoe_measurement_max_exposure_per_frame '1200.0 s'
_stoe_measurement_mean_exposure_per_frame '1200.0 s'
_stoe_measurement_min_exposure_per_frame '1200.0 s'
_stoe_measurement_total_exposure_time '109.7 h'
_stoe_measurement_total_frame_number 329
_stoe_measurement_total_run_number 2
_stoe_measurement_tube_power     '1.5 kW'