#------------------------------------------------------------------------------
#$Date: 2022-09-19 02:08:58 +0300 (Mon, 19 Sep 2022) $
#$Revision: 277972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/12/7711288.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_7711288
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         'C8 H22 Al2 Cl2 P2'
_chemical_formula_sum            'C8 H22 Al2 Cl2 P2'
_chemical_formula_weight         305.05
_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             2022-05-19
_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                76.9990(10)
_cell_angle_beta                 70.5430(10)
_cell_angle_gamma                66.6410(10)
_cell_formula_units_Z            1
_cell_length_a                   6.5589(2)
_cell_length_b                   7.5892(2)
_cell_length_c                   9.2977(2)
_cell_measurement_reflns_used    3959
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.66
_cell_measurement_theta_min      2.34
_cell_volume                     398.300(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.928
_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_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8302
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.740
_diffrn_reflns_theta_min         2.941
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1381 before and 0.0413 after correction.
 
For component 2:
 wR2(int) was 0.1090 before and 0.0453 after correction.
 
For component 3:
 wR2(int) was 0.1324 before and 0.0446 after correction.
 The Ratio of minimum to maximum transmission is 0.89.

Final HKLF 4 output contains 58476 reflections, Rint = 0.0371
 (36614 with I > 3sig(I), Rint = 0.0313)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       plate
_exptl_crystal_F_000             160
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         8302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0408P)²+0.0595P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7151
_reflns_number_total             8302
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02519a2.cif
_cod_data_source_block           PAlMeCl
_cod_database_code               7711288
_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   0.947
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.45369
 0.26294 0.28337
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_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
Cl1 Cl 0.29109(6) 0.33384(5) 0.30295(4) 0.02261(10) Uani 1 1 d . . . . .
P1 P 0.51138(6) 0.29929(5) 0.67655(4) 0.01291(9) Uani 1 1 d . . . . .
Al1 Al 0.61070(7) 0.35854(6) 0.30509(5) 0.01369(10) Uani 1 1 d . . . . .
C1 C 0.6468(3) 0.1581(2) 0.82786(17) 0.0228(3) Uani 1 1 d . . . . .
H1A H 0.788728 0.182414 0.813264 0.034 Uiso 1 1 calc R U . . .
H1B H 0.683984 0.020500 0.823920 0.034 Uiso 1 1 calc R U . . .
H1C H 0.540432 0.195359 0.927834 0.034 Uiso 1 1 calc R U . . .
C2 C 0.2686(3) 0.2222(2) 0.71050(17) 0.0206(3) Uani 1 1 d . . . . .
H2A H 0.165320 0.249978 0.813114 0.031 Uiso 1 1 calc R U . . .
H2B H 0.325284 0.083170 0.703270 0.031 Uiso 1 1 calc R U . . .
H2C H 0.184323 0.291877 0.633441 0.031 Uiso 1 1 calc R U . . .
C3 C 0.7069(2) 0.22277(19) 0.49526(15) 0.0151(2) Uani 1 1 d . . . . .
H3A H 0.737594 0.083620 0.497631 0.018 Uiso 1 1 calc R U . . .
H3B H 0.854915 0.236005 0.486427 0.018 Uiso 1 1 calc R U . . .
C4 C 0.8495(2) 0.3015(2) 0.10907(14) 0.0150(2) Uani 1 1 d . . . . .
H4A H 0.886288 0.168359 0.091446 0.023 Uiso 1 1 calc R U . . .
H4B H 0.988829 0.317194 0.112896 0.023 Uiso 1 1 calc R U . . .
H4C H 0.792304 0.390440 0.025311 0.023 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 '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'
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
C1 P1 Al1 110.47(5) . 2_666 ?
C2 P1 Al1 112.12(5) . 2_666 ?
C2 P1 C1 103.75(7) . . ?
C3 P1 Al1 114.44(5) . 2_666 ?
C3 P1 C1 108.43(7) . . ?
C3 P1 C2 107.02(7) . . ?
Cl1 Al1 P1 101.36(2) . 2_666 ?
C3 Al1 Cl1 112.40(4) . . ?
C3 Al1 P1 106.12(4) . 2_666 ?
C4 Al1 Cl1 111.57(4) . . ?
C4 Al1 P1 107.64(4) . 2_666 ?
C4 Al1 C3 116.35(6) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C3 Al1 117.90(7) . . ?
P1 C3 H3A 107.8 . . ?
P1 C3 H3B 107.8 . . ?
Al1 C3 H3A 107.8 . . ?
Al1 C3 H3B 107.8 . . ?
H3A C3 H3B 107.2 . . ?
Al1 C4 H4A 109.5 . . ?
Al1 C4 H4B 109.5 . . ?
Al1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
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
Cl1 Al1 2.1843(5) . ?
P1 Al1 2.4234(5) 2_666 ?
P1 C1 1.8208(15) . ?
P1 C2 1.8158(14) . ?
P1 C3 1.7979(14) . ?
Al1 C3 1.9984(14) . ?
Al1 C4 1.9693(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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 P1 C3 Al1 -54.15(8) 2_666 . . . ?
C1 P1 C3 Al1 -177.95(7) . . . . ?
C2 P1 C3 Al1 70.70(9) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.45369
2 0.26294
3 0.28337
