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_7244337
_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         'C39 H47 N4 P'
_chemical_formula_sum            'C39 H49 N4 P'
_chemical_formula_weight         604.79
_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   mixed
_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                101.570(2)
_cell_angle_beta                 100.081(2)
_cell_angle_gamma                111.127(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4611(2)
_cell_length_b                   12.4141(3)
_cell_length_c                   16.7883(4)
_cell_measurement_reflns_used    11807
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      28.6720
_cell_measurement_theta_min      2.9910
_cell_volume                     1734.64(8)
_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      249.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.875
_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    -54.00  36.00   0.50   10.00    --    7.20 -38.00 150.00  180
  2  \w    -19.00  31.00   0.50   10.00    --    7.20 -57.00  30.00  100
  3  \w    -70.00  37.00   0.50   10.00    --    7.20 -57.00  60.00  214
  4  \w    -80.00 -54.00   0.50   10.00    --    7.20 -57.00  30.00   52
  5  \w    -87.00  17.00   0.50   10.00    --   -7.60 -57.00 120.00  208
  6  \w    -97.00  -7.00   0.50   10.00    --   -7.60 -57.00 -60.00  180
  7  \w    -62.00  20.00   0.50   10.00    --   -7.60 -82.00 -90.00  164
;
_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      0.0481428000
_diffrn_orient_matrix_UB_12      0.0284175000
_diffrn_orient_matrix_UB_13      0.0421101000
_diffrn_orient_matrix_UB_21      -0.0183949000
_diffrn_orient_matrix_UB_22      -0.0571764000
_diffrn_orient_matrix_UB_23      0.0073680000
_diffrn_orient_matrix_UB_31      0.0656829000
_diffrn_orient_matrix_UB_32      -0.0035105000
_diffrn_orient_matrix_UB_33      -0.0133902000
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27111
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.908
_diffrn_reflns_theta_min         2.617
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76682
_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    1.158
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0690P)^2^+0.3066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6548
_reflns_number_total             8000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00242f2.cif
_cod_data_source_block           1b
_cod_original_cell_volume        1734.64(7)
_cod_database_code               7244337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNP
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C3(H3), C20(H20), C39(H39), C18(H18), C4(H4), C5(H5), C27(H27),
 C29(H29), C36(H36), C37(H37), C38(H38), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C22(H22A,H22B,H22C),
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              35009
_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 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.601