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_7244336
_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         '0.25(C29 H43 N4 P), 0.13(C4 H8)'
_chemical_formula_sum            'C7.75 H11.75 N P0.25'
_chemical_formula_weight         126.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.693(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   10.4218(5)
_cell_length_b                   14.9253(7)
_cell_length_c                   20.5378(9)
_cell_measurement_reflns_used    8453
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3390
_cell_measurement_theta_min      2.9100
_cell_volume                     3139.2(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.883
_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     53.00  91.00   0.50   64.79    --    7.10  77.00-150.00   76
  2  \w    -11.00  21.00   0.50   64.79    --   -7.50 -57.00-180.00   64
  3  \w    -36.00  20.00   0.50   64.79    --   -7.50  57.00   0.00  112
  4  \w    -64.00 -38.00   0.50   64.79    --   -7.50 -57.00-180.00   52
  5  \w    -54.00   8.00   0.50   64.79    --   -7.50 -82.00-180.00  124
  6  \w    -95.00  26.00   0.50   64.79    --   -7.50  19.00 150.00  242
;
_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      -0.0114925000
_diffrn_orient_matrix_UB_12      -0.0113422000
_diffrn_orient_matrix_UB_13      0.0319560000
_diffrn_orient_matrix_UB_21      -0.0044820000
_diffrn_orient_matrix_UB_22      0.0461409000
_diffrn_orient_matrix_UB_23      0.0075385000
_diffrn_orient_matrix_UB_31      -0.0681720000
_diffrn_orient_matrix_UB_32      -0.0010694000
_diffrn_orient_matrix_UB_33      -0.0125114000
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28830
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.981
_diffrn_reflns_theta_min         2.729
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71528
_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    1.072
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0899
_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/[\s^2^(Fo^2^)+(0.1605P)^2^+1.7995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2664
_refine_ls_wR_factor_ref         0.2856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5144
_reflns_number_total             7361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00242f2.cif
_cod_data_source_block           1c
_cod_database_code               7244336
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNP
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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 Secondary CH2 refined with riding coordinates:
 C00Z(H00A,H00B), C010(H01A,H01B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C4(H4), C15(H15), C29(H29), C25(H25), C27(H27),
 C28(H28), C26(H26)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C8(H8A,H8B,
 H8C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              9239
_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 1.662
_oxdiff_exptl_absorpt_empirical_full_min 0.667