New zinc complexes derived from “self-adaptable” acyclic diiminodipyrromethanes as potent catalysts for the reduction of curing temperature of bisphenol-A/F benzoxazines
Loke, Shiva K.; Pagadala, Eswar; Devaraju, S.; Srinivasadesikan, V.; Kottalanka, Ravi K.; RSC Advances 10 (2020) 36275–36286; doi:10.1039/D0RA07837A

data_7241339
_publ_section_title
;
 New zinc complexes derived from &#x201C;self-adaptable&#x201D; acyclic
 diiminodipyrromethanes as potent catalysts for the reduction of curing
 temperature of bisphenol-A/F benzoxazines
;
_journal_issue                   60
_journal_name_full               'RSC Advances'
_journal_page_first              36275
_journal_page_last               36286
_journal_paper_doi               10.1039/D0RA07837A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C56 H46 Cl2 N4 Zn, C7 H8'
_chemical_formula_sum            'C63 H54 Cl2 N4 Zn'
_chemical_formula_weight         1003.46
_chemical_name_systematic        ZnCl2N4C63H54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-12 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                85.646(2)
_cell_angle_beta                 89.156(2)
_cell_angle_gamma                73.944(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8769(3)
_cell_length_b                   13.4192(4)
_cell_length_c                   17.2498(4)
_cell_measurement_reflns_used    14885
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      73.9700
_cell_measurement_theta_min      4.4050
_cell_volume                     2634.32(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9941
_diffrn_measured_fraction_theta_max 0.9581
_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    -10.00  17.00   0.50   10.00    --    0.00 -57.00  60.00   54
  2  \w    -32.00  16.00   0.50   10.00    --    0.00 -37.00 -30.00   96
  3  \w    -22.00  50.00   0.50   10.00    --    0.00  57.00-120.00  144
  4  \w    -88.00 -36.00   0.50   10.00    --    0.00 -37.00 -30.00  104
  5  \w    -72.00 -47.00   0.50   10.00    --    0.00 -57.00  60.00   50
  6  \w      0.00  26.00   0.50   10.00    --    0.00  37.00-180.00   52
  7  \w     16.00  84.00   0.50   10.00    --    0.00  37.00 -60.00  136
  8  \w     63.00  88.00   0.50   10.00    --    0.00  57.00-120.00   50
  9  \w     87.00 113.00   0.50   10.00    --   95.80 -82.00 -90.00   52
 10  \w      7.00 115.00   0.50   10.00    --   95.80 -30.00 -30.00  216
 11  \w     12.00  85.00   0.50   10.00    --   95.80 -15.00-150.00  146
 12  \w    141.00 184.00   0.50   10.00    --   95.80  61.00 -60.00   86
 13  \w     76.00 121.00   0.50   10.00    --   95.80  45.00   0.00   90
 14  \w     66.00 106.00   0.50   10.00    --   95.80 -82.00 150.00   80
 15  \w     68.00 176.00   0.50   10.00    --   95.80  15.00 120.00  216
 16  \w     17.00  44.00   0.50   10.00    --   95.80 -82.00 150.00   54
 17  \w      9.00 120.00   0.50   10.00    --   95.80 -61.00-150.00  222
 18  \w     18.00  91.00   0.50   10.00    --   95.80 -61.00 120.00  146
 19  \w     52.00 127.00   0.50   10.00    --   95.80 -82.00   0.00  150
 20  \w     85.00 124.00   0.50   10.00    --   95.80 -82.00  60.00   78
 21  \w     10.00 127.00   0.50   10.00    --   95.80 -82.00-150.00  234
 22  \w     20.00 119.00   0.50   10.00    --   95.80 -61.00   0.00  198
 23  \w     86.00 120.00   0.50   10.00    --   95.80  30.00   0.00   68
 24  \w    144.00 170.00   0.50   10.00    --   95.80  30.00   0.00   52
 25  \w     97.00 122.00   0.50   10.00    --   95.80 -15.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0362430000
_diffrn_orient_matrix_UB_12      0.0639232000
_diffrn_orient_matrix_UB_13      -0.0780977000
_diffrn_orient_matrix_UB_21      -0.1204773000
_diffrn_orient_matrix_UB_22      0.0529182000
_diffrn_orient_matrix_UB_23      0.0340534000
_diffrn_orient_matrix_UB_31      0.0488960000
_diffrn_orient_matrix_UB_32      0.0864009000
_diffrn_orient_matrix_UB_33      0.0276370000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26749
_diffrn_reflns_theta_full        74.4658
_diffrn_reflns_theta_max         74.47
_diffrn_reflns_theta_min         4.14
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2650
_exptl_crystal_description       block
_exptl_crystal_F_000             1048.8798
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.2754
_refine_diff_density_min         -0.8652
_refine_diff_density_rms         0.0870
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             10.6897
_refine_ls_goodness_of_fit_ref   1.0445
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    79
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0445
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.0021
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+3.0042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8926
_reflns_number_total             10280
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0ra07837a2.cif
_cod_data_source_block           exp_356_a_2
_cod_database_code               7241339
_chemical_oxdiff_usercomment     'PALE YELLOW BLOCK'
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C4)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8ba), C59(H59), C11(H2aa), C54(H48), C41(H41), C23(H31), C22(H32),
 C16(H2ba), C53(H47), C40(H40), C30(H24), C56(H50), C29(H23), C35(H35),
 C24(H30), C17(H0ba), C20(H7aa), C26(H28), C34(H34), C19(H8aa), C25(H29),
 C18(H9aa), C52(H46), C28(H22), C44(H44), C62(H62), C13(H4aa), C32(H26),
 C31(H25), C63(H63), C55(H49), C60(H60), C4(H4ba), C43(H43), C61(H61)
3.b Idealised Me refined as rotating group:
 C57(H57a,H57b,H57c), C1(H0aa,H0ab,H0ac)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.791
_oxdiff_exptl_absorpt_empirical_full_min 0.661