#------------------------------------------------------------------------------
#$Date: 2022-09-19 02:08:58 +0300 (Mon, 19 Sep 2022) $
#$Revision: 277972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/12/7711290.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7711290
loop_
_publ_author_name
'Paskaruk, Katarina'
'Emslie, David J. H.'
'Britten, James F.'
_publ_section_title
;
 Coordination chemistry and structural rearrangements of the Me2PCH2AlMe2
 ambiphilic ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02519A
_journal_year                    2022
_chemical_formula_moiety         'C22 H60 Al2 P6 Pt2'
_chemical_formula_sum            'C22 H60 Al2 P6 Pt2'
_chemical_formula_weight         954.66
_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             2022-05-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                103.209(2)
_cell_angle_beta                 107.622(2)
_cell_angle_gamma                105.478(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4084(3)
_cell_length_b                   9.6824(3)
_cell_length_c                   11.1418(4)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      36.084
_cell_measurement_theta_min      8.45
_cell_volume                     877.82(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            85463
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.589
_diffrn_reflns_theta_min         2.318
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.294
_exptl_absorpt_correction_T_max  0.2716
_exptl_absorpt_correction_T_min  0.1921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0740 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.7073.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         9849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0194P)²+0.0324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9154
_reflns_number_total             9849
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02519a2.cif
_cod_data_source_block           PtPPPAlMe
_cod_original_cell_volume        877.82(5)
_cod_database_code               7711290
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.317
_shelx_estimated_absorpt_t_min   0.263
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7A,H7B), C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C),
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.16782(5) 0.23526(5) 0.40305(4) 0.01284(7) Uani 1 1 d . . . . .
C4 C 0.32408(16) 0.22528(15) 0.56921(13) 0.0141(2) Uani 1 1 d . . . . .
H4A H 0.286648 0.119242 0.568543 0.017 Uiso 1 1 calc R U . . .
H4B H 0.428295 0.244730 0.559838 0.017 Uiso 1 1 calc R U . . .
C7 C 0.23368(17) 0.45001(15) 0.39617(14) 0.0164(2) Uani 1 1 d . . . . .
H7A H 0.151141 0.491863 0.406278 0.020 Uiso 1 1 calc R U . . .
H7B H 0.334901 0.513533 0.473932 0.020 Uiso 1 1 calc R U . . .
C10 C 0.18432(16) 0.09351(15) 0.24678(14) 0.0155(2) Uani 1 1 d . . . . .
H10A H 0.177249 -0.003730 0.263537 0.019 Uiso 1 1 calc R U . . .
H10B H 0.089326 0.071349 0.165778 0.019 Uiso 1 1 calc R U . . .
C11 C -0.05850(17) 0.15867(18) 0.38463(17) 0.0207(3) Uani 1 1 d . . . . .
H11A H -0.079428 0.066702 0.409484 0.031 Uiso 1 1 calc R U . . .
H11B H -0.129579 0.134603 0.291733 0.031 Uiso 1 1 calc R U . . .
H11C H -0.078117 0.236924 0.443606 0.031 Uiso 1 1 calc R U . . .
C3 C 0.4292(2) 0.25990(17) 0.85533(15) 0.0211(3) Uani 1 1 d . . . . .
H3A H 0.354587 0.155049 0.826302 0.032 Uiso 1 1 calc R U . . .
H3B H 0.433731 0.317826 0.941804 0.032 Uiso 1 1 calc R U . . .
H3C H 0.535994 0.259525 0.864262 0.032 Uiso 1 1 calc R U . . .
C2 C 0.16079(18) 0.31811(18) 0.73152(17) 0.0213(3) Uani 1 1 d . . . . .
H2A H 0.105722 0.362918 0.670498 0.032 Uiso 1 1 calc R U . . .
H2B H 0.169265 0.366655 0.822104 0.032 Uiso 1 1 calc R U . . .
H2C H 0.099997 0.208720 0.701867 0.032 Uiso 1 1 calc R U . . .
C6 C 0.24718(17) 0.65329(16) 0.24410(16) 0.0193(3) Uani 1 1 d . . . . .
H6A H 0.152884 0.661431 0.261010 0.029 Uiso 1 1 calc R U . . .
H6B H 0.237447 0.661507 0.156143 0.029 Uiso 1 1 calc R U . . .
H6C H 0.343541 0.735444 0.313255 0.029 Uiso 1 1 calc R U . . .
C5 C 0.07031(17) 0.35083(17) 0.10718(16) 0.0205(3) Uani 1 1 d . . . . .
H5A H 0.058515 0.243441 0.086927 0.031 Uiso 1 1 calc R U . . .
H5B H 0.068211 0.380518 0.028444 0.031 Uiso 1 1 calc R U . . .
H5C H -0.017850 0.365646 0.131187 0.031 Uiso 1 1 calc R U . . .
C8 C 0.30961(18) 0.01784(17) 0.04582(15) 0.0202(3) Uani 1 1 d . . . . .
H8A H 0.282266 -0.085162 0.050741 0.030 Uiso 1 1 calc R U . . .
H8B H 0.402006 0.041021 0.020388 0.030 Uiso 1 1 calc R U . . .
H8C H 0.218223 0.024178 -0.021142 0.030 Uiso 1 1 calc R U . . .
C9 C 0.50284(18) 0.10346(17) 0.32406(16) 0.0195(2) Uani 1 1 d . . . . .
H9A H 0.540434 0.174514 0.415046 0.029 Uiso 1 1 calc R U . . .
H9B H 0.593921 0.108513 0.297636 0.029 Uiso 1 1 calc R U . . .
H9C H 0.451543 -0.000232 0.321331 0.029 Uiso 1 1 calc R U . . .
C1 C 0.33626(17) 0.66225(16) 0.80223(16) 0.0181(2) Uani 1 1 d . . . . .
H1A H 0.250645 0.634940 0.714851 0.027 Uiso 1 1 calc R U . . .
H1B H 0.377101 0.772618 0.847266 0.027 Uiso 1 1 calc R U . . .
H1C H 0.294115 0.610428 0.856930 0.027 Uiso 1 1 calc R U . . .
P1 P 0.36105(4) 0.34801(4) 0.73168(4) 0.01302(6) Uani 1 1 d . . . . .
P2 P 0.26152(4) 0.46865(4) 0.24767(4) 0.01267(5) Uani 1 1 d . . . . .
P3 P 0.35872(4) 0.15483(4) 0.20891(4) 0.01299(6) Uani 1 1 d . . . . .
Pt1 Pt 0.52388(2) 0.59485(2) 0.77554(2) 0.01108(1) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Al1 C7 110.27(6) . . ?
C4 Al1 C10 105.35(6) . . ?
C10 Al1 C7 109.10(6) . . ?
C11 Al1 C4 113.54(6) . . ?
C11 Al1 C7 111.32(6) . . ?
C11 Al1 C10 106.95(6) . . ?
Al1 C4 H4A 107.3 . . ?
Al1 C4 H4B 107.3 . . ?
H4A C4 H4B 106.9 . . ?
P1 C4 Al1 120.13(7) . . ?
P1 C4 H4A 107.3 . . ?
P1 C4 H4B 107.3 . . ?
Al1 C7 H7A 108.3 . . ?
Al1 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
P2 C7 Al1 115.98(7) . . ?
P2 C7 H7A 108.3 . . ?
P2 C7 H7B 108.3 . . ?
Al1 C10 H10A 107.7 . . ?
Al1 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
P3 C10 Al1 118.43(7) . . ?
P3 C10 H10A 107.7 . . ?
P3 C10 H10B 107.7 . . ?
Al1 C11 H11A 109.5 . . ?
Al1 C11 H11B 109.5 . . ?
Al1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P3 C8 H8A 109.5 . . ?
P3 C8 H8B 109.5 . . ?
P3 C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P3 C9 H9A 109.5 . . ?
P3 C9 H9B 109.5 . . ?
P3 C9 H9C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Pt1 C1 H1A 109.5 . . ?
Pt1 C1 H1B 109.5 . . ?
Pt1 C1 H1C 109.5 . . ?
C4 P1 C3 108.89(7) . . ?
C4 P1 C2 103.65(7) . . ?
C4 P1 Pt1 111.71(4) . . ?
C3 P1 C2 98.04(8) . . ?
C3 P1 Pt1 115.74(5) . . ?
C2 P1 Pt1 117.39(5) . . ?
C7 P2 C6 104.92(7) . . ?
C7 P2 C5 106.52(7) . . ?
C7 P2 Pt1 112.56(5) . 2_666 ?
C6 P2 Pt1 121.45(5) . 2_666 ?
C5 P2 C6 96.36(7) . . ?
C5 P2 Pt1 113.09(5) . 2_666 ?
C10 P3 C8 104.76(7) . . ?
C10 P3 C9 102.40(7) . . ?
C10 P3 Pt1 121.91(5) . 2_666 ?
C8 P3 Pt1 113.04(5) . 2_666 ?
C9 P3 C8 103.38(7) . . ?
C9 P3 Pt1 109.40(5) . 2_666 ?
C1 Pt1 P1 87.05(4) . . ?
C1 Pt1 P2 177.47(4) . 2_666 ?
C1 Pt1 P3 84.91(4) . 2_666 ?
P1 Pt1 P2 95.235(12) . 2_666 ?
P1 Pt1 P3 168.543(12) . 2_666 ?
P3 Pt1 P2 92.982(12) 2_666 2_666 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 C4 2.0267(14) . ?
Al1 C7 2.0315(14) . ?
Al1 C10 2.0310(15) . ?
Al1 C11 1.9873(15) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 P1 1.7959(14) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 P2 1.7923(14) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 P3 1.7991(14) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 P1 1.8251(15) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 P1 1.8277(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 P2 1.8368(14) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 P2 1.8362(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 P3 1.8269(15) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 P3 1.8249(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 Pt1 2.1152(13) . ?
P1 Pt1 2.3144(3) . ?
P2 Pt1 2.3297(3) 2_666 ?
P3 Pt1 2.3211(3) 2_666 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 C4 P1 C3 155.06(8) . . . . ?
Al1 C4 P1 C2 51.45(9) . . . . ?
Al1 C4 P1 Pt1 -75.87(8) . . . . ?
Al1 C7 P2 C6 160.19(8) . . . . ?
Al1 C7 P2 C5 58.73(9) . . . . ?
Al1 C7 P2 Pt1 -65.75(8) . . . 2_666 ?
Al1 C10 P3 C8 -168.56(8) . . . . ?
Al1 C10 P3 C9 83.81(9) . . . . ?
Al1 C10 P3 Pt1 -38.71(10) . . . 2_666 ?
