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_7062097
_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         'C25 H23 N3 O4 Zn, C3 H5 N'
_chemical_formula_sum            'C28 H28 N4 O4 Zn'
_chemical_formula_weight         549.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                90
_cell_angle_beta                 96.5300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.57440(10)
_cell_length_b                   24.2668(4)
_cell_length_c                   10.97570(10)
_cell_measurement_reflns_used    27469
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.0470
_cell_measurement_theta_min      3.1070
_cell_volume                     2533.55(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.959
_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    -16.00  88.00   1.00   25.00    --   14.05  57.00-180.00  104
  2  \w    -60.00  44.00   1.00   25.00    --   14.05 -57.00 -90.00  104
  3  \w    -42.00  48.00   1.00   25.00    --   14.05 -77.00  30.00   90
  4  \w    -15.00  56.00   1.00   25.00    --   14.05 -99.00 150.00   71
  5  \w    -12.00  90.00   1.00   25.00    --   14.05  37.00 -30.00  102
  6  \w    -16.00  88.00   1.00   25.00    --   14.05  57.00  60.00  104
  7  \w    -48.00  21.00   1.00   25.00    --  -14.36  77.00-150.00   69
  8  \w    -42.00  19.00   1.00   25.00    --  -14.36 -77.00-180.00   61
  9  \w     49.00  96.00   1.00   25.00    --   14.05 167.00 -61.00   47
 10  \w    -89.00 -41.00   1.00   25.00    --  -14.36 151.00  27.27   48
 11  \w    -77.00 -33.00   1.00   25.00    --  -14.36 133.00 121.44   44
 12  \w    -89.00 -41.00   1.00   25.00    --  -14.36 152.00 174.12   48
 13  \w    -72.00 -27.00   1.00   25.00    --  -14.36 125.00   1.78   45
 14  \w    -76.00 -30.00   1.00   25.00    --  -14.36 132.00 -59.89   46
 15  \w     39.00  89.00   1.00   25.00    --   14.05 178.00 -60.00   50
 16  \w    -91.00 -43.00   1.00   25.00    --  -14.36 154.00-135.38   48
;
_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      -0.0702362000
_diffrn_orient_matrix_UB_12      -0.0093462000
_diffrn_orient_matrix_UB_13      -0.0003581000
_diffrn_orient_matrix_UB_21      -0.0247491000
_diffrn_orient_matrix_UB_22      0.0272978000
_diffrn_orient_matrix_UB_23      -0.0111537000
_diffrn_orient_matrix_UB_31      -0.0039198000
_diffrn_orient_matrix_UB_32      -0.0046952000
_diffrn_orient_matrix_UB_33      -0.0640701000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37001
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.310
_diffrn_reflns_theta_min         2.300
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62116
_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    1.442
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3138 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.3307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                6796
_reflns_number_total             6999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04668g2.cif
_cod_data_source_block           1CH3CH2CN
_cod_depositor_comments
'Adding full bibliography for 7062097--7062109.cif.'
_cod_database_code               7062097
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.632
_reflns_odcompleteness_completeness 99.93
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C42(H42A,H42B)
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)
2.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              27428
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.314
_oxdiff_exptl_absorpt_empirical_full_min 0.592