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_7062104
_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         '2(C15 H17 N2 O2 Zn0.5), 2.5(C7 H5 N)'
_chemical_formula_sum            'C47.5 H46.5 N6.5 O4 Zn'
_chemical_formula_weight         837.78
_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             2022-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-28 deposited with the CCDC.	2022-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.319(3)
_cell_angle_beta                 97.791(2)
_cell_angle_gamma                97.798(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6600(2)
_cell_length_b                   14.7528(5)
_cell_length_c                   18.8900(6)
_cell_measurement_reflns_used    14689
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.0620
_cell_measurement_theta_min      2.6320
_cell_volume                     2093.56(11)
_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 0.898
_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    -14.00  88.00   1.00    7.50    --   14.05  57.00 120.00  102
  2  \w      0.00  44.00   1.00    7.50    --   14.05 -57.00 120.00   44
  3  \w    -42.00  48.00   1.00    7.50    --   14.05 -77.00  90.00   90
  4  \w    -41.00  48.00   1.00    7.50    --   14.05 -77.00 -30.00   89
  5  \w     -3.00  89.00   1.00    7.50    --   14.05  37.00  30.00   92
  6  \w    -14.00  88.00   1.00    7.50    --   14.05  57.00-120.00  102
  7  \w    -42.00  48.00   1.00    7.50    --   14.05 -77.00-120.00   90
  8  \w    -36.00  13.00   1.00    7.50    --  -14.36 -77.00-120.00   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      -0.0324086000
_diffrn_orient_matrix_UB_12      0.0082470000
_diffrn_orient_matrix_UB_13      0.0326513000
_diffrn_orient_matrix_UB_21      -0.0123830000
_diffrn_orient_matrix_UB_22      0.0448611000
_diffrn_orient_matrix_UB_23      -0.0103373000
_diffrn_orient_matrix_UB_31      -0.0877856000
_diffrn_orient_matrix_UB_32      -0.0166915000
_diffrn_orient_matrix_UB_33      -0.0163070000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37788
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.312
_diffrn_reflns_theta_min         2.537
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53399
_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    1.329
_exptl_crystal_description       needle
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11268
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0334P)^2^+0.7497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9346
_reflns_number_total             11268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04668g2.cif
_cod_data_source_block           225PhCN
_cod_depositor_comments
'Adding full bibliography for 7062097--7062109.cif.'
_cod_original_formula_sum        'C47.50 H46.50 N6.50 O4 Zn'
_cod_database_code               7062104
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.700
_reflns_odcompleteness_completeness 99.95
_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. Rigid body (RIGU) restrains
 N6, C61, C62, C63, C67, C64, C66, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61A, N6A, C62A, C63A, C67A, C64A, C66A, C65A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(N6A)=Sof(C61A)=Sof(C62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=Sof(H67A)=1-FVAR(1)
 Sof(N6)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=FVAR(1)
 Fixed Sof: N7(0.5) C71(0.5) C72(0.5) C73(0.5) H73(0.5) C74(0.5) H74(0.5)
 C75(0.5) H75(0.5) C76(0.5) H76(0.5) C77(0.5) H77(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
 C45(H45A,H45B)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
 C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A), C67A(H67A), C73(H73), C74(H74),
  C75(H75), C76(H76), C77(H77)
;
_shelx_res_checksum              60411
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.547
_oxdiff_exptl_absorpt_empirical_full_min 0.427