From cyclic amines and acetonitrile to amidine zinc(ii) complexes
Podjed, Nina; Modec, Barbara; Alcaide, María M.; López-Serrano, Joaquín; RSC Advances 10 (2020) 18200–18221; doi:10.1039/D0RA03192E

data_7240521
_publ_section_title
;
 From cyclic amines and acetonitrile to amidine zinc(ii) complexes
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              18200
_journal_page_last               18221
_journal_paper_doi               10.1039/D0RA03192E
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C30 H18 N3 O6 Zn, C7 H15 N2'
_chemical_formula_sum            'C37 H33 N5 O6 Zn'
_chemical_formula_weight         709.05
_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
_audit_creation_date             2019-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-19 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                88.709(2)
_cell_angle_beta                 88.368(2)
_cell_angle_gamma                82.441(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5111(2)
_cell_length_b                   12.6993(3)
_cell_length_c                   13.6361(3)
_cell_measurement_reflns_used    17889
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.1850
_cell_measurement_theta_min      3.1910
_cell_volume                     1631.76(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_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 1.000
_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      0.00  25.00   1.00    1.00    --   38.00  93.00-111.92   25
  2  \w    -47.00 -13.00   1.00    1.00    --  -41.63 -57.00-120.00   34
  3  \w   -107.00 -17.00   1.00    1.00    --  -41.63 -37.00 120.00   90
  4  \w    -64.00  33.00   1.00    1.00    --  -41.63  37.00-150.00   97
  5  \w    -91.00  -3.00   1.00    1.00    --  -41.63 125.00-150.00   88
  6  \w   -115.00 -66.00   1.00    1.00    --  -41.63 -57.00-120.00   49
  7  \w   -101.00 -18.00   1.00    1.00    --  -41.63 -37.00  30.00   83
  8  \w     23.00  96.00   1.00    1.00    --   41.63-125.00  60.00   73
  9  \w      7.00  32.00   1.00    1.00    --   42.00  86.00 101.36   25
 10  \w     16.00  43.00   1.00    1.00    --   50.00  81.00 -84.36   27
 11  \w     18.00  44.00   1.00    1.00    --   50.00  79.00 121.23   26
 12  \w     16.00  41.00   1.00    1.00    --   50.00  82.00 -15.97   25
 13  \w     27.00  56.00   1.00    1.00    --   58.00  76.00  34.95   29
 14  \w     91.00 120.00   1.00    1.00    --   62.00  76.00-170.65   29
 15  \w     32.00  58.00   1.00    1.00    --   62.00  76.00-170.65   26
 16  \w     32.00  58.00   1.00    1.00    --   62.00  75.00 154.50   26
 17  \w     34.00  62.00   1.00    1.00    --   66.00  76.00 -12.09   28
 18  \w     34.00  59.00   1.00    1.00    --   66.00  77.00 -58.78   25
 19  \w    102.00 142.00   1.00    1.00    --   70.00  76.00-133.94   40
 20  \w    118.00 143.00   1.00    1.00    --   70.00  75.00-101.02   25
 21  \w    110.00 144.00   1.00    1.00    --   70.00  75.00 114.81   34
 22  \w     38.00  64.00   1.00    1.00    --   70.00  75.00-101.02   26
 23  \w     38.00  64.00   1.00    1.00    --   70.00  76.00-133.94   26
 24  \w     38.00  76.00   1.00    1.00    --   70.00  75.00 114.81   38
 25  \w     37.00  71.00   1.00    1.00    --   70.00  77.00  56.69   34
 26  \w     42.00  71.00   1.00    1.00    --   74.00  73.00 -74.14   29
 27  \w     44.00  84.00   1.00    1.00    --   74.00  77.00  19.64   40
 28  \w     54.00  80.00   1.00    2.00    --   82.00  54.00 177.78   26
 29  \w     59.00  90.00   1.00    2.00    --   86.00  55.00  71.62   31
 30  \w     53.00  80.00   1.00    2.00    --   86.00  77.00 -12.93   27
 31  \w     63.00  89.00   1.00    2.00    --   90.00  59.00 -46.56   26
 32  \w     58.00  84.00   1.00    2.00    --   90.00  73.00 168.01   26
 33  \w    149.00 174.00   1.00    2.00    --  102.00  66.00 -80.79   25
 34  \w     73.00  99.00   1.00    2.00    --  102.00  66.00 -80.79   26
 35  \w     40.00 128.00   1.00    2.00    --  109.50 -61.00-180.00   88
 36  \w     80.00 106.00   1.00    2.00    --  109.50  61.00-150.00   26
 37  \w    109.00 168.00   1.00    2.00    --  109.50  66.00-172.16   59
 38  \w     36.00 115.00   1.00    2.00    --  109.50-125.00 120.00   79
 39  \w     81.00 106.00   1.00    2.00    --  109.50  61.00  90.00   25
 40  \w     79.00 105.00   1.00    2.00    --  109.50  66.00-172.16   26
 41  \w    108.00 178.00   1.00    2.00    --  109.50  77.00   0.00   70
 42  \w     77.00 103.00   1.00    2.00    --  109.50  77.00   0.00   26
 43  \w     28.00 107.00   1.00    2.00    --  109.50 -94.00-180.00   79
 44  \w     78.00 177.00   1.00    2.00    --  109.50  77.00 150.00   99
 45  \w     84.00 109.00   1.00    2.00    --  109.50 -94.00-150.00   25
 46  \w     77.00 177.00   1.00    2.00    --  109.50  77.00  60.00  100
 47  \w     77.00 168.00   1.00    2.00    --  109.50  77.00 -30.00   91
 48  \w     77.00 146.00   1.00    2.00    --  109.50  77.00-120.00   69
 49  \w     77.00 172.00   1.00    2.00    --  109.50  77.00  30.00   95
 50  \w    119.00 144.00   1.00    2.00    --  109.50  61.00-120.00   25
 51  \w     77.00 173.00   1.00    2.00    --  109.50  77.00 120.00   96
 52  \w    117.00 148.00   1.00    2.00    --  109.50  77.00  90.00   31
 53  \w     48.00  86.00   1.00    2.00    --  109.50 -94.00   0.00   38
 54  \w     61.00 117.00   1.00    2.00    --  109.50-125.00-180.00   56
 55  \w     86.00 111.00   1.00    2.00    --  109.50  61.00-120.00   25
 56  \w     77.00 111.00   1.00    2.00    --  109.50  77.00  90.00   34
 57  \w     81.00 108.00   1.00    2.00    --  109.50  61.00  30.00   27
 58  \w     84.00 111.00   1.00    2.00    --  109.50  61.00 120.00   27
 59  \w     77.00 133.00   1.00    2.00    --  109.50  77.00-150.00   56
 60  \w     27.00  77.00   1.00    2.00    --  109.50 -94.00 120.00   50
 61  \w     77.00 168.00   1.00    2.00    --  109.50  77.00 -90.00   91
 62  \w     57.00 117.00   1.00    2.00    --  109.50-125.00  90.00   60
 63  \w     38.00 117.00   1.00    2.00    --  109.50-125.00   0.00   79
 64  \w     77.00 145.00   1.00    2.00    --  109.50  77.00 -60.00   68
;
_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      0.1237934000
_diffrn_orient_matrix_UB_12      -0.0381287000
_diffrn_orient_matrix_UB_13      -0.0713489000
_diffrn_orient_matrix_UB_21      -0.1066458000
_diffrn_orient_matrix_UB_22      -0.0151982000
_diffrn_orient_matrix_UB_23      -0.0797772000
_diffrn_orient_matrix_UB_31      0.0041530000
_diffrn_orient_matrix_UB_32      0.1153087000
_diffrn_orient_matrix_UB_33      -0.0363828000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29230
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.980
_diffrn_reflns_theta_min         3.243
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0526P)^2^+0.7068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5975
_reflns_number_total             6194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra03192e3.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7240517--7240533.cif.
;
_cod_database_code               7240521
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.583
_shelx_res_checksum              61337