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_4348169
_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         'C16 H24 N4 O2 Zn, C3 H8 O'
_chemical_formula_sum            'C19 H32 N4 O3 Zn'
_chemical_formula_weight         429.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            4
_cell_length_a                   8.95087(10)
_cell_length_b                   12.63503(10)
_cell_length_c                   19.02315(15)
_cell_measurement_reflns_used    13235
_cell_measurement_temperature    200
_cell_measurement_theta_max      72.4710
_cell_measurement_theta_min      3.4510
_cell_volume                     2151.41(3)
_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)'
_computing_structure_solution    'ShelXS (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 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -50.00   36.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680   38.0000  -90.0000 215

  2 omega -122.00    6.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -19.0000  -90.0000 320

  3 omega   27.00   99.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0680 -129.0000  -89.0000 180

  4 omega   28.00   90.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000    0.0000 155

  5 omega   28.00   90.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000   60.0000 155

  6 omega   21.00  107.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -94.0000  -90.0000 215

  7 omega   28.00   90.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000  -90.0000 155

  8 omega   31.00  135.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -61.0000 -150.0000 260

  9 omega   28.00   90.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000  -60.0000 155

 10 omega   28.00   90.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000 -180.0000 155

 11 omega   21.00  107.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -94.0000    0.0000 215

 12 omega -119.00   -7.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -77.0000  -90.0000 280

 13 omega -114.00  -10.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -57.0000  150.0000 260

 14 omega -114.00  -10.00   0.4000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -57.0000   60.0000 260

 15 omega   75.00  177.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   30.0000 -120.0000 255

 16 omega   44.00  178.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   15.0000  120.0000 335

 17 omega   75.00  177.00   0.4000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   61.0000  -30.0000 255
;
_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      -0.0079398000
_diffrn_orient_matrix_UB_12      -0.0974679000
_diffrn_orient_matrix_UB_13      0.0485639000
_diffrn_orient_matrix_UB_21      -0.0145490000
_diffrn_orient_matrix_UB_22      -0.0724886000
_diffrn_orient_matrix_UB_23      -0.0648212000
_diffrn_orient_matrix_UB_31      0.1711211000
_diffrn_orient_matrix_UB_32      -0.0108152000
_diffrn_orient_matrix_UB_33      -0.0032253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19788
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.475
_diffrn_reflns_theta_min         4.200
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.798
_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    1.327
_exptl_crystal_description
;
;
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.2953
_exptl_crystal_size_mid          0.0511
_exptl_crystal_size_min          0.0383
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1715 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0347P)^2^+0.4708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                4089
_reflns_number_total             4202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01066_si_002.cif
_cod_data_source_block           9b-str1633
_cod_original_cell_volume        2151.42(3)
_cod_database_code               4348169
_chemical_oxdiff_formula         'C16 H24 N4 O2 Zn'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C10(H10), C11(H11), C14(H14), C18(H18)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;