#------------------------------------------------------------------------------
#$Date: 2022-09-19 02:08:58 +0300 (Mon, 19 Sep 2022) $
#$Revision: 277972 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/12/7711287.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_7711287
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 H40 P2 Rh2'
_chemical_formula_sum            'C22 H40 P2 Rh2'
_chemical_formula_weight         572.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-12
_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                90
_cell_angle_beta                 93.2420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1428(7)
_cell_length_b                   6.3491(3)
_cell_length_c                   19.3303(12)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.05
_cell_measurement_theta_min      2.25
_cell_volume                     2223.10(19)
_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 0.979
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47952
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.724
_diffrn_reflns_theta_min         2.110
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0435 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.9316.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         4333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0295P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3672
_reflns_number_total             4333
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02519a2.cif
_cod_data_source_block           RhcodCH2PMe2
_cod_database_code               7711287
_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   0.908
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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
Rh1 Rh 0.33574(2) 0.42815(2) 0.58196(2) 0.00827(3) Uani 1 1 d . . . . .
P1 P 0.28978(2) 0.49365(5) 0.41714(2) 0.00915(6) Uani 1 1 d . . . . .
C1 C 0.33750(7) 0.6136(2) 0.49156(6) 0.0107(2) Uani 1 1 d . . . . .
H1A H 0.314484 0.751676 0.500453 0.013 Uiso 1 1 calc R U . . .
H1B H 0.389458 0.639584 0.480922 0.013 Uiso 1 1 calc R U . . .
C2 C 0.34467(7) 0.2607(2) 0.39869(7) 0.0149(2) Uani 1 1 d . . . . .
H2A H 0.396559 0.301229 0.396038 0.022 Uiso 1 1 calc R U . . .
H2B H 0.326615 0.199304 0.354411 0.022 Uiso 1 1 calc R U . . .
H2C H 0.340245 0.156910 0.435738 0.022 Uiso 1 1 calc R U . . .
C3 C 0.31316(7) 0.6633(2) 0.34403(7) 0.0165(3) Uani 1 1 d . . . . .
H3A H 0.283008 0.791400 0.343929 0.025 Uiso 1 1 calc R U . . .
H3B H 0.303361 0.587229 0.300365 0.025 Uiso 1 1 calc R U . . .
H3C H 0.365540 0.701468 0.348956 0.025 Uiso 1 1 calc R U . . .
C4 C 0.44453(6) 0.3004(2) 0.55858(6) 0.0117(2) Uani 1 1 d . . . . .
H4 H 0.459401 0.331689 0.510617 0.014 Uiso 1 1 calc R U . . .
C5 C 0.45524(7) 0.4662(2) 0.60456(6) 0.0114(2) Uani 1 1 d . . . . .
H5 H 0.476393 0.595247 0.583592 0.014 Uiso 1 1 calc R U . . .
C6 C 0.47613(7) 0.4398(2) 0.68124(7) 0.0138(2) Uani 1 1 d . . . . .
H6A H 0.510428 0.554116 0.696471 0.017 Uiso 1 1 calc R U . . .
H6B H 0.502340 0.304165 0.688569 0.017 Uiso 1 1 calc R U . . .
C7 C 0.40838(7) 0.4442(2) 0.72599(7) 0.0145(2) Uani 1 1 d . . . . .
H7A H 0.421021 0.371275 0.770346 0.017 Uiso 1 1 calc R U . . .
H7B H 0.396580 0.592469 0.736780 0.017 Uiso 1 1 calc R U . . .
C8 C 0.34066(7) 0.3412(2) 0.69127(6) 0.0126(2) Uani 1 1 d . . . . .
H8 H 0.293983 0.368853 0.714882 0.015 Uiso 1 1 calc R U . . .
C9 C 0.33962(7) 0.1568(2) 0.65229(7) 0.0138(2) Uani 1 1 d . . . . .
H9 H 0.291807 0.078574 0.652746 0.017 Uiso 1 1 calc R U . . .
C10 C 0.40605(7) 0.0144(2) 0.64270(7) 0.0158(2) Uani 1 1 d . . . . .
H10A H 0.389017 -0.133555 0.639307 0.019 Uiso 1 1 calc R U . . .
H10B H 0.440493 0.026031 0.684117 0.019 Uiso 1 1 calc R U . . .
C11 C 0.44793(8) 0.0688(2) 0.57769(7) 0.0151(2) Uani 1 1 d . . . . .
H11A H 0.500291 0.027142 0.585812 0.018 Uiso 1 1 calc R U . . .
H11B H 0.426883 -0.014827 0.538106 0.018 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 '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 Rh1 P1 88.10(3) . 2_556 ?
C1 Rh1 C4 88.85(5) . . ?
C1 Rh1 C5 92.42(5) . . ?
C1 Rh1 C8 160.46(5) . . ?
C1 Rh1 C9 161.94(5) . . ?
C4 Rh1 P1 163.71(3) . 2_556 ?
C5 Rh1 P1 159.54(3) . 2_556 ?
C5 Rh1 C4 36.63(5) . . ?
C8 Rh1 P1 91.41(3) . 2_556 ?
C8 Rh1 C4 96.75(5) . . ?
C8 Rh1 C5 81.35(5) . . ?
C8 Rh1 C9 37.11(5) . . ?
C9 Rh1 P1 97.67(3) . 2_556 ?
C9 Rh1 C4 80.82(5) . . ?
C9 Rh1 C5 88.09(5) . . ?
C1 P1 Rh1 119.82(4) . 2_556 ?
C1 P1 C2 104.76(6) . . ?
C1 P1 C3 104.08(6) . . ?
C2 P1 Rh1 113.75(4) . 2_556 ?
C2 P1 C3 99.87(6) . . ?
C3 P1 Rh1 112.28(4) . 2_556 ?
Rh1 C1 H1A 108.9 . . ?
Rh1 C1 H1B 108.9 . . ?
P1 C1 Rh1 113.31(6) . . ?
P1 C1 H1A 108.9 . . ?
P1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
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 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Rh1 C4 H4 114.1 . . ?
C5 C4 Rh1 71.54(7) . . ?
C5 C4 H4 114.1 . . ?
C5 C4 C11 125.36(12) . . ?
C11 C4 Rh1 109.35(8) . . ?
C11 C4 H4 114.1 . . ?
Rh1 C5 H5 113.9 . . ?
C4 C5 Rh1 71.82(7) . . ?
C4 C5 H5 113.9 . . ?
C4 C5 C6 124.12(12) . . ?
C6 C5 Rh1 111.73(8) . . ?
C6 C5 H5 113.9 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
C5 C6 C7 112.50(10) . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 C6 113.30(11) . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
Rh1 C8 H8 114.1 . . ?
C7 C8 Rh1 107.93(8) . . ?
C7 C8 H8 114.1 . . ?
C9 C8 Rh1 71.93(7) . . ?
C9 C8 C7 126.08(11) . . ?
C9 C8 H8 114.1 . . ?
Rh1 C9 H9 113.5 . . ?
C8 C9 Rh1 70.95(7) . . ?
C8 C9 H9 113.5 . . ?
C8 C9 C10 125.26(12) . . ?
C10 C9 Rh1 112.82(9) . . ?
C10 C9 H9 113.5 . . ?
C9 C10 H10A 108.9 . . ?
C9 C10 H10B 108.9 . . ?
C9 C10 C11 113.24(11) . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C4 C11 C10 113.57(11) . . ?
C4 C11 H11A 108.9 . . ?
C4 C11 H11B 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
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
Rh1 P1 2.3161(3) 2_556 ?
Rh1 C1 2.1091(12) . ?
Rh1 C4 2.2041(12) . ?
Rh1 C5 2.2006(12) . ?
Rh1 C8 2.1807(12) . ?
Rh1 C9 2.1932(13) . ?
P1 C1 1.8050(12) . ?
P1 C2 1.8291(13) . ?
P1 C3 1.8456(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4 1.0000 . ?
C4 C5 1.3843(18) . ?
C4 C11 1.5168(18) . ?
C5 H5 1.0000 . ?
C5 C6 1.5184(18) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.5428(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.5147(18) . ?
C8 H8 1.0000 . ?
C8 C9 1.3921(19) . ?
C9 H9 1.0000 . ?
C9 C10 1.5263(18) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.5440(19) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
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
Rh1 P1 C1 Rh1 62.81(7) 2_556 . . . ?
Rh1 C4 C5 C6 104.37(12) . . . . ?
Rh1 C4 C11 C10 -35.41(13) . . . . ?
Rh1 C5 C6 C7 -13.19(13) . . . . ?
Rh1 C8 C9 C10 104.98(12) . . . . ?
Rh1 C9 C10 C11 -10.30(14) . . . . ?
C2 P1 C1 Rh1 -66.31(7) . . . . ?
C3 P1 C1 Rh1 -170.72(6) . . . . ?
C4 C5 C6 C7 -95.39(14) . . . . ?
C5 C4 C11 C10 45.25(17) . . . . ?
C5 C6 C7 C8 35.87(15) . . . . ?
C6 C7 C8 Rh1 -39.92(13) . . . . ?
C6 C7 C8 C9 40.43(18) . . . . ?
C7 C8 C9 Rh1 -99.38(12) . . . . ?
C7 C8 C9 C10 5.6(2) . . . . ?
C8 C9 C10 C11 -92.47(15) . . . . ?
C9 C10 C11 C4 30.70(16) . . . . ?
C11 C4 C5 Rh1 -101.04(12) . . . . ?
C11 C4 C5 C6 3.33(19) . . . . ?
