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_4348172
_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         'C12 H12 N2 Ni0.5 O'
_chemical_formula_sum            'C12 H11 N Ni0.5 O2'
_chemical_formula_weight         230.57
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.81680(10)
_cell_length_b                   11.81680(10)
_cell_length_c                   14.84740(18)
_cell_measurement_reflns_used    11112
_cell_measurement_temperature    200
_cell_measurement_theta_max      72.4850
_cell_measurement_theta_min      3.7510
_cell_volume                     2073.24(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      200
_diffrn_detector_area_resol_mean 20.8101
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -129.00  -35.80   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930  178.0000  120.0000 233

  2 omega  -29.00   33.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930   38.0000    0.0000 155

  3 omega  -29.00   18.20   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930   38.0000 -180.0000 118

  4 omega  -46.00  -20.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000    0.0000 65

  5 omega   87.00  117.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   45.0000  120.0000 75

  6 omega   72.00   98.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -45.0000  120.0000 65

  7 omega   28.00   90.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000 -120.0000 155

  8 omega   28.00   85.20   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000 -180.0000 143

  9 omega   39.00   90.20   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -45.0000    0.0000 128

 10 omega   59.00   93.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -45.0000  -60.0000 85

 11 omega   16.00  160.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400    0.0000  -60.0000 360

 12 omega -114.00  -12.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930  -57.0000   30.0000 255

 13 omega -114.00  -12.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930  -57.0000  120.0000 255

 14 omega -119.00   -7.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930  -77.0000 -120.0000 280

 15 omega -140.00  -28.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000  -30.0000 280

 16 omega   72.00  178.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   77.0000  120.0000 265

 17 omega   75.00  177.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   61.0000   60.0000 255

 18 omega   75.00  177.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   30.0000    0.0000 255

 19 omega   72.00  144.80   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   77.0000 -120.0000 182

 20 omega   31.00  121.00   0.4000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      105.5400 -125.0000 -150.0000 225
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0520447000
_diffrn_orient_matrix_UB_12      0.0949249000
_diffrn_orient_matrix_UB_13      -0.0577823000
_diffrn_orient_matrix_UB_21      -0.0009012000
_diffrn_orient_matrix_UB_22      0.0794912000
_diffrn_orient_matrix_UB_23      0.0822417000
_diffrn_orient_matrix_UB_31      0.1195550000
_diffrn_orient_matrix_UB_32      -0.0406881000
_diffrn_orient_matrix_UB_33      0.0258213000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19255
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.497
_diffrn_reflns_theta_min         4.783
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94610
_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    1.477
_exptl_crystal_description
;
;
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.2616
_exptl_crystal_size_mid          0.2186
_exptl_crystal_size_min          0.1611
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 789 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(8)
_refine_ls_extinction_coef       0.0018(2)
_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   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0325P)^2^+0.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.655
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                2021
_reflns_number_total             2060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01066_si_002.cif
_cod_data_source_block           10c-str1603
_cod_original_formula_sum        'C12 H11 N Ni0.50 O2'
_cod_database_code               4348172
_chemical_oxdiff_formula         'C24 H26 N4 O2 Ni'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 N(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
;