Cu(2+), Zn(2+), and Ni(2+) Complexes of C2-Symmetric Pseudopeptides with an Aromatic Central Spacer.
Gorla, Lingaraju; Martí-Centelles, Vicente; Freimuth, Lena; Altava, Belén; Burguete, M. Isabel; Luis, Santiago V.; Inorganic chemistry 55 (2016) 7617–7629; doi:10.1021/acs.inorgchem.6b01066

data_4348167
_publ_section_title
;
 Cu(2+), Zn(2+), and Ni(2+) Complexes of C2-Symmetric Pseudopeptides with
 an Aromatic Central Spacer.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7617
_journal_page_last               7629
_journal_paper_doi               10.1021/acs.inorgchem.6b01066
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C24 H26 N4 O2'
_chemical_formula_sum            'C24 H26 N4 O2'
_chemical_formula_weight         402.49
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                71.785(2)
_cell_angle_beta                 88.7145(19)
_cell_angle_gamma                76.039(2)
_cell_formula_units_Z            4
_cell_length_a                   8.6682(2)
_cell_length_b                   14.7652(3)
_cell_length_c                   18.3708(4)
_cell_measurement_reflns_used    39195
_cell_measurement_temperature    200
_cell_measurement_theta_max      71.9560
_cell_measurement_theta_min      4.6960
_cell_volume                     2163.86(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega -116.00   -5.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000  -90.0000 138

  2 omega  -49.00   41.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   37.0000   60.0000 113

  3 omega -117.00   -6.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -37.0000  -30.0000 138

  4 omega -117.00   -6.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -37.0000   90.0000 138

  5 omega -129.00  -34.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  178.0000   30.0000 118

  6 omega   55.00  127.80   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057 -178.0000   30.0000 91

  7 omega   -1.00   31.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   90.0000   60.7022 40

  8 omega   10.00   38.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   84.0000 -129.3630 35

  9 omega   15.00   44.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000   65.4405 37

 10 omega   20.00   45.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   79.0000  -17.8599 32

 11 omega   19.00   44.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   80.0000 -167.1049 32

 12 omega   19.00   44.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   81.0000  135.6723 32

 13 omega   20.00   45.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   79.0000  -67.5239 32

 14 omega   28.00  146.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   76.0000   12.4936 148

 15 omega   32.00  150.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000   98.6769 148

 16 omega   33.00  149.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   70.0000  -89.1364 145

 17 omega   36.00  156.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000   61.9062 150

 18 omega   36.00  154.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   76.0000  -49.6636 148

 19 omega   37.00  153.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   69.0000 -157.5191 145

 20 omega   37.00  153.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   69.0000 -114.9638 145

 21 omega   36.00  150.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   65.0000  162.8482 143

 22 omega   41.00  157.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   70.0000 -136.1438 145

 23 omega   43.00  153.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   57.0000  -53.1773 138

 24 omega   61.00  177.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   71.0000  -58.7092 145

 25 omega   69.00  177.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0000   66.0000   53.9114 135

 26 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000 -120.0000 133

 27 omega   20.00  108.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000 -180.0000 110

 28 omega   74.00  178.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000    0.0000 130

 29 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000    0.0000 133

 30 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000  120.0000 133

 31 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000  150.0000 133

 32 omega   20.00  108.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000  -30.0000 110

 33 omega   20.00  108.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000   90.0000 110

 34 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000 -180.0000 133

 35 omega   28.00   96.80   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -45.0000   60.0000 86

 36 omega   20.00  108.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000  -90.0000 110

 37 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000  -60.0000 133

 38 omega   72.00  177.60   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   63.0000  146.9907 132

 39 omega   20.00  108.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524  -94.0000   30.0000 110

 40 omega   74.00  178.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000   30.0000 130

 41 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000   90.0000 133

 42 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000  -30.0000 133

 43 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000 -150.0000 133

 44 omega   72.00  177.60   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   64.0000  -27.7043 132

 45 omega   71.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   77.0000   60.0000 133

 46 omega   73.00  177.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000  -92.5995 130

 47 omega   57.00  129.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  178.0000 -180.0000 90

 48 omega    5.00  115.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057   57.0000 -180.0000 138

 49 omega    4.00   32.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   89.0000 -173.7188 35

 50 omega   15.00   43.80   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000 -162.3339 36

 51 omega   15.00   44.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   81.0000  -49.3580 37

 52 omega   22.00  138.80   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   74.0000  -83.0484 146

 53 omega   19.00   43.80   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   82.0000   75.2791 31

 54 omega   24.00  144.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000 -137.6583 150

 55 omega   24.00  142.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   76.0000  117.5651 148

 56 omega   29.00  142.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   63.0000 -169.1280 142

 57 omega   28.00  148.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000   52.7337 150

 58 omega   32.00  150.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000   65.8602 148

 59 omega   32.00  150.40   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000  -58.8833 148

 60 omega   32.00  152.00   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  -18.4387 150

 61 omega   40.00  149.60   0.8000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   51.0000   66.6514 137

 62 omega   74.00  178.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000 -180.0000 130

 63 omega   74.00  178.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000  120.0000 130

 64 omega   74.00  178.00   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   61.0000 -120.0000 130

 65 omega   75.00  177.40   0.8000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7524   51.0000  116.4109 128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0998480000
_diffrn_orient_matrix_UB_12      0.0396442000
_diffrn_orient_matrix_UB_13      -0.0675367000
_diffrn_orient_matrix_UB_21      0.1444976000
_diffrn_orient_matrix_UB_22      -0.0857997000
_diffrn_orient_matrix_UB_23      0.0372905000
_diffrn_orient_matrix_UB_31      -0.0529225000
_diffrn_orient_matrix_UB_32      -0.0625579000
_diffrn_orient_matrix_UB_33      -0.0432200000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72792
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.171
_diffrn_reflns_theta_min         3.433
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description
;
;
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.2458
_exptl_crystal_size_mid          0.1942
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 6291 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(14)
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         16019
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.7701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                14702
_reflns_number_total             16019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01066_si_002.cif
_cod_data_source_block           6a-str1720
_cod_original_cell_volume        2163.85(9)
_cod_database_code               4348167
_chemical_oxdiff_formula         'C24 H26 N4 O2'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H2AB-N2A
 0.9 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C1D(H1D), C10D(H10D), C1C(H1C), C10C(H10C), C1A(H1A), C10A(H10A), C1B(H1B),
 C10B(H10B)
3.b Secondary CH2 refined with riding coordinates:
 C11D(H11A,H11B), C18D(H18A,H18B), C11C(H11C,H11D), C18C(H18C,H18D), C11A(H11E,
 H11F), C18A(H18E,H18F), C11B(H11G,H11H), C18B(H18G,H18H)
3.c Aromatic/amide H refined with riding coordinates:
 C4D(H4D), C5D(H5D), C6D(H6D), C7D(H7D), C13D(H13D), C14D(H14D), C15D(H15D),
 C16D(H16D), C17D(H17D), C20D(H20D), C21D(H21D), C22D(H22D), C23D(H23D),
 C24D(H24D), C4C(H4C), C5C(H5C), C6C(H6C), C7C(H7C), C13C(H13C), C14C(H14C),
 C15C(H15C), C16C(H16C), C17C(H17C), C20C(H20C), C21C(H21C), C22C(H22C),
 C23C(H23C), C24C(H24C), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A), C13A(H13A),
 C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C20A(H20A), C21A(H21A),
 C22A(H22A), C23A(H23A), C24A(H24A), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C20B(H20B),
 C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B)
;