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_4348171
_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 H24 Cu N4 O2'
_chemical_formula_sum            'C24 H24 Cu N4 O2'
_chemical_formula_weight         464.01
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                81.1495(17)
_cell_angle_beta                 67.742(2)
_cell_angle_gamma                62.348(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1351(2)
_cell_length_b                   10.5175(2)
_cell_length_c                   11.9667(2)
_cell_measurement_reflns_used    15577
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      72.5500
_cell_measurement_theta_min      3.9730
_cell_volume                     1045.34(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -23.00   24.60   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   38.0000 -180.0000 68

  2 omega -118.00   19.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -19.0000    0.0000 197

  3 omega   96.00  127.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  178.0000   90.0000 45

  4 omega  -52.00   -3.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   45.0000   30.0000 70

  5 omega  -44.00    5.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   30.0000  -30.0000 70

  6 omega -148.00 -118.60   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000 -111.0000  -60.0000 42

  7 omega   79.00  174.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   30.0000  150.0000 137

  8 omega   23.00   81.10   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -94.0000 -120.0000 83

  9 omega   28.00   81.20   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -30.0000 -120.0000 76

 10 omega   21.00  104.30   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -94.0000  -60.0000 119

 11 omega  139.00  174.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   30.0000 -120.0000 51

 12 omega   46.00   81.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -45.0000    0.0000 50

 13 omega   30.00  109.10   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  -94.0000    0.0000 113

 14 omega  143.00  171.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  102.0000 -147.0000 41

 15 omega   72.00  149.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  178.0000 -120.0000 110

 16 omega  103.00  131.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308  111.0000  -30.0000 40

 17 omega   76.00  171.20   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   61.0000   30.0000 136

 18 omega   32.00  115.30   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000 -150.0000 119

 19 omega -122.00   -1.60   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000  -30.0000 172

 20 omega  -49.00   42.00   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   38.0000   90.0000 130

 21 omega -122.00   -1.60   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000  120.0000 172

 22 omega -116.00   -4.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000 -150.0000 159

 23 omega -153.00  -31.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -77.0000 -180.0000 173

 24 omega -153.00  -31.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -77.0000    0.0000 173

 25 omega -153.00  -31.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -77.0000  -90.0000 173

 26 omega -153.00  -31.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -77.0000   90.0000 173

 27 omega   77.00  178.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   45.0000   90.0000 145

 28 omega   75.00  177.90   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   61.0000  -30.0000 147

 29 omega   72.00  177.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   77.0000  -90.0000 151

 30 omega   27.00  178.20   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   15.0000  -60.0000 216

 31 omega   28.00  115.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308 -111.0000   90.0000 125

 32 omega   72.00  177.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   77.0000   30.0000 151

 33 omega   72.00  177.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   77.0000 -150.0000 151

 34 omega   72.00  177.70   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   77.0000  150.0000 151

 35 omega -122.00   -1.60   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000 -150.0000 172

 36 omega -116.00   -6.10   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -38.0000  -30.0000 157

 37 omega   72.00  131.50   0.7000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3308   77.0000  120.0000 85
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0708888000
_diffrn_orient_matrix_UB_12      0.0715232000
_diffrn_orient_matrix_UB_13      0.1257233000
_diffrn_orient_matrix_UB_21      -0.1128184000
_diffrn_orient_matrix_UB_22      0.1378551000
_diffrn_orient_matrix_UB_23      -0.0442325000
_diffrn_orient_matrix_UB_31      -0.1258434000
_diffrn_orient_matrix_UB_32      -0.0569645000
_diffrn_orient_matrix_UB_33      0.0400025000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17715
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.729
_diffrn_reflns_theta_min         3.993
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description
;
;
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.5105
_exptl_crystal_size_mid          0.3314
_exptl_crystal_size_min          0.1669
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 3240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0569P)^2^+0.1223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.834
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                7369
_reflns_number_total             7408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01066_si_002.cif
_cod_data_source_block           10a-str1599
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H48 Cu2 N8 O4'
_cod_original_formula_weight         928.02
_cod_original_formula_moiety         '2(C24 H24 Cu N4 O2)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1045.35(5)
_cod_database_code               4348171
_chemical_oxdiff_formula         'C H N O Cu'
_reflns_odcompleteness_completeness 100.00
_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, All N(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1A(H1A), C10A(H10A), C1B(H1B), C10B(H10B)
2.b Secondary CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N2A(H2AA,H2AB), C11A(H11A,H11B), C18A(H18A,H18B), N1B(H1BA,
 H1BB), N2B(H2BA,H2BB), C11B(H11C,H11D), C18B(H18C,H18D)
2.c Aromatic/amide H refined with riding coordinates:
 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)
;