Amidines from cyclic amines and nitriles in the presence of zinc(ii): other nitriles in place of acetonitrile
Podjed, Nina; Modec, Barbara; New Journal of Chemistry 46 (2022) 23225–23238; doi:10.1039/D2NJ04668G

data_7062107
_publ_section_title
;
 Amidines from cyclic amines and nitriles in the presence of zinc(ii):
 other nitriles in place of acetonitrile
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              23225
_journal_page_last               23238
_journal_paper_doi               10.1039/D2NJ04668G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C31 H26 N4 O4 Zn'
_chemical_formula_sum            'C31 H26 N4 O4 Zn'
_chemical_formula_weight         583.93
_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             2022-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-05 deposited with the CCDC.	2022-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                94.937(2)
_cell_angle_beta                 90.8110(10)
_cell_angle_gamma                90.7760(10)
_cell_formula_units_Z            4
_cell_length_a                   10.1047(2)
_cell_length_b                   15.6035(3)
_cell_length_c                   16.7005(3)
_cell_measurement_reflns_used    27754
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.9830
_cell_measurement_theta_min      2.6680
_cell_volume                     2622.83(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4933
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.936
_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     39.00 104.00   1.00   15.00    --   14.05 178.00-120.00   65
  2  \w    -42.00  48.00   1.00   15.00    --   14.05 -77.00  90.00   90
  3  \w    -16.00  88.00   1.00   15.00    --   14.05  57.00-120.00  104
  4  \w    -16.00  88.00   1.00   15.00    --   14.05  57.00 120.00  104
  5  \w    -60.00  44.00   1.00   15.00    --   14.05 -57.00 -30.00  104
  6  \w    -12.00  90.00   1.00   15.00    --   14.05  37.00  30.00  102
  7  \w    -42.00  19.00   1.00   15.00    --  -14.36 -77.00-120.00   61
  8  \w    -48.00  21.00   1.00   15.00    --  -14.36  77.00-120.00   69
  9  \w    -74.00 -30.00   1.00   15.00    --  -14.36 128.00 148.50   44
 10  \w     25.00  94.00   1.00   15.00    --   14.05-160.00  -3.00   69
 11  \w    -76.00 -30.00   1.00   15.00    --  -14.36 132.00 110.13   46
 12  \w    -74.00 -30.00   1.00   15.00    --  -14.36 128.00-160.45   44
 13  \w    -77.00 -33.00   1.00   15.00    --  -14.36 133.00 -36.31   44
 14  \w    -94.00 -46.00   1.00   15.00    --  -14.36 159.00  26.64   48
 15  \w    -42.00  -1.00   1.00   15.00    --  -14.36 -77.00-180.00   41
 16  \w    -93.00 -44.00   1.00   15.00    --  -14.36 156.00 -86.93   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159037000
_diffrn_orient_matrix_UB_12      -0.0011478000
_diffrn_orient_matrix_UB_13      0.0413940000
_diffrn_orient_matrix_UB_21      -0.0284952000
_diffrn_orient_matrix_UB_22      0.0410592000
_diffrn_orient_matrix_UB_23      0.0081948000
_diffrn_orient_matrix_UB_31      -0.0621650000
_diffrn_orient_matrix_UB_32      -0.0198776000
_diffrn_orient_matrix_UB_33      0.0060931000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            77591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.260
_diffrn_reflns_theta_min         2.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         14668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0376P)^2^+1.6827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11968
_reflns_number_total             14668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04668g2.cif
_cod_data_source_block           9a
_cod_depositor_comments
'Adding full bibliography for 7062097--7062109.cif.'
_cod_database_code               7062107
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56),
 C57(H57), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C73(H73),
  C74(H74), C75(H75), C76(H76), C77(H77)
;
_shelx_res_checksum              89699
_shelx_fab_checksum              77679
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.790