Aluminium alkyl complexes supported by imino-phosphanamide ligand as precursors for catalytic guanylation reactions of carbodiimides
Karmakar, Himadri; Anga, Srinivas; Panda, Tarun K.; Chandrasekhar, Vadapalli; RSC Advances 12 (2022) 4501–4509; doi:10.1039/D2RA00242F

data_7244339
_publ_section_title
;
 Aluminium alkyl complexes supported by imino-phosphanamide ligand as
 precursors for catalytic guanylation reactions of carbodiimides
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4501
_journal_page_last               4509
_journal_paper_doi               10.1039/D2RA00242F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         '2(C41 H52 Al N4 P), C3 H3'
_chemical_formula_sum            'C85 H107 Al2 N8 P2'
_chemical_formula_weight         1356.68
_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             2021-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                99.080(2)
_cell_angle_beta                 91.255(2)
_cell_angle_gamma                100.416(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2350(2)
_cell_length_b                   19.8700(3)
_cell_length_c                   20.5541(4)
_cell_measurement_reflns_used    31142
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      27.7680
_cell_measurement_theta_min      2.7860
_cell_volume                     4054.20(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -46.00 -21.00   0.50   32.37    --    7.20 -56.00 -34.00   50
  2  \w     -6.00  97.00   0.50   32.37    --    7.20  56.00 107.00  206
  3  \w     22.00  47.00   0.50   32.37    --   -7.60  56.00 107.00   50
  4  \w    -61.00 -36.00   0.50   32.37    --   -7.60 -56.00 -34.00   50
  5  \w    -82.00  97.00   0.50   32.37    --    7.20  19.00  60.00  358
  6  \w    -58.00 -32.00   0.50   32.37    --    7.20 -38.00-150.00   52
  7  \w     -6.00  20.00   0.50   32.37    --    7.20 -38.00-150.00   52
  8  \w    -61.00 -35.00   0.50   32.37    --    7.20 -82.00  90.00   52
  9  \w    -15.00  11.00   0.50   32.37    --    7.20 -82.00  90.00   52
 10  \w     -2.00  24.00   0.50   32.37    --    7.20  57.00  60.00   52
 11  \w    -82.00  38.00   0.50   32.37    --    7.20 -57.00-150.00  240
 12  \w    -48.00 -23.00   0.50   32.37    --    7.20  19.00   0.00   50
 13  \w     23.00  49.00   0.50   32.37    --    7.20  19.00   0.00   52
 14  \w    -60.00  36.00   0.50   32.37    --   -7.60 -82.00-180.00  192
 15  \w    -50.00 -22.00   0.50   32.37    --   -7.60 -82.00 -60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0566250000
_diffrn_orient_matrix_UB_12      0.0016245000
_diffrn_orient_matrix_UB_13      -0.0193858000
_diffrn_orient_matrix_UB_21      -0.0185689000
_diffrn_orient_matrix_UB_22      0.0277979000
_diffrn_orient_matrix_UB_23      -0.0135597000
_diffrn_orient_matrix_UB_31      0.0377786000
_diffrn_orient_matrix_UB_32      0.0240546000
_diffrn_orient_matrix_UB_33      0.0257857000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.080
_diffrn_reflns_theta_min         2.641
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         19084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0628P)^2^+0.7250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14961
_reflns_number_total             19084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00242f2.cif
_cod_data_source_block           2b
_cod_database_code               7244339
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNPAl
_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.a Ternary CH refined with riding coordinates:
 C50(H50), C12(H12), C9(H9), C53(H53)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C31(H31), C29(H29), C78(H78), C41(H41), C38(H38), C46(H46),
 C48(H48), C85(H85), C47(H47), C63(H63), C84(H84), C20(H20), C40(H40), C83(H83),
  C61(H61), C17(H17), C82(H82), C70(H70), C39(H39), C6(H6), C16(H16), C7(H7),
 C22(H22), C5(H5), C72(H72), C58(H58), C57(H57), C79(H79), C81(H81), C80(H80)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C35(H35A,H35B,H35C), C51(H51A,H51B,H51C), C42(H42A,H42B,
 H42C), C2(H2A,H2B,H2C), C43(H43A,H43B,H43C), C33(H33A,H33B,H33C), C67(H67A,
 H67B,H67C), C52(H52A,H52B,H52C), C13(H13A,H13B,H13C), C26(H26A,H26B,H26C),
 C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C74(H74A,H74B,H74C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C76(H76A,H76B,H76C), C10(H10A,H10B,H10C), C11(H11A,
 H11B,H11C), C75(H75A,H75B,H75C), C55(H55A,H55B,H55C), C14(H14A,H14B,H14C),
 C54(H54A,H54B,H54C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              25499
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.738