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_4348168
_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         '2(C16 H24 Cu N4 O2), 2(H2 O)'
_chemical_formula_sum            'C32 H52 Cu2 N8 O6'
_chemical_formula_weight         771.89
_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                   11.2386(3)
_cell_length_b                   15.6641(3)
_cell_length_c                   21.5505(5)
_cell_measurement_reflns_used    10519
_cell_measurement_temperature    200
_cell_measurement_theta_max      72.4890
_cell_measurement_theta_min      3.4620
_cell_volume                     3793.81(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega -124.00  -67.60   0.6000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930    0.0000 -180.0000 94

  2 omega  -20.00   22.00   0.6000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930    0.0000 -180.0000 70

  3 omega  -49.00    7.40   0.6000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930   38.0000 -150.0000 94

  4 omega   35.80   90.40   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000    0.0000 91

  5 omega  124.00  174.40   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  114.0000  -32.0000 84

  6 omega   23.00   98.00   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -94.0000  120.0000 125

  7 omega   49.00  137.80   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -77.0000  -90.0000 148

  8 omega -114.00  -12.00   0.6000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930  -57.0000   60.0000 170

  9 omega  -50.00   34.60   0.6000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1930   38.0000    0.0000 141

 10 omega   75.00  177.00   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   30.0000   30.0000 170

 11 omega   78.00  107.40   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   45.0000  -60.0000 49

 12 omega   44.00  176.60   0.6000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   15.0000 -180.0000 221
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0653227000
_diffrn_orient_matrix_UB_12      0.0203008000
_diffrn_orient_matrix_UB_13      -0.0611920000
_diffrn_orient_matrix_UB_21      0.0351477000
_diffrn_orient_matrix_UB_22      -0.0946362000
_diffrn_orient_matrix_UB_23      -0.0062544000
_diffrn_orient_matrix_UB_31      -0.1154372000
_diffrn_orient_matrix_UB_32      -0.0172167000
_diffrn_orient_matrix_UB_33      -0.0363378000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18518
_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         72.536
_diffrn_reflns_theta_min         3.488
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57481
_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    1.351
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.3612
_exptl_crystal_size_mid          0.3314
_exptl_crystal_size_min          0.2276
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_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     541
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0966P)^2^+0.5655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.699
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                6627
_reflns_number_total             7042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01066_si_002.cif
_cod_data_source_block           9a-str1602
_cod_original_cell_volume        3793.80(16)
_cod_database_code               4348168
_chemical_oxdiff_formula         'C16 H26 N4 O2 Cu'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H,H,H,H,H,H,H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2A-O2 = O2-H2B
 0.85 with sigma of 0.02
 H1E-O1 = O1-H1F
 0.85 with sigma of 0.02
 H2BB-N2B
 0.91 with sigma of 0.02
 H1BA-N1B
 0.91 with sigma of 0.02
 N1B-H1BB
 0.91 with sigma of 0.02
 N2B-H2BA
 0.91 with sigma of 0.02
 N1A-H1AA
 0.91 with sigma of 0.02
 N1A-H1AB
 0.91 with sigma of 0.02
 N2A-H2AA
 0.91 with sigma of 0.02
 H2AB-N2A
 0.91 with sigma of 0.02
 H2A-H2B
 1.367 with sigma of 0.04
 H1E-H1F
 1.367 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C12B)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C13B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C12A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C12B)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C13B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Sof(H1AD)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5C)=Sof(H5D)=Sof(H5E)=Sof(C6)=Sof(H6C)=
 Sof(H6D)=Sof(H6E)=1-FVAR(1)
 Sof(H1AC)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=FVAR(1)
 Sof(H1BC)=Sof(C1)=Sof(H1A)=Sof(H1C)=Sof(H1D)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(H3C)=1-FVAR(2)
 Sof(H1B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13B)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C1B(H1B), C1B(H1BC), C10B(H10B), C14B(H14B), C11B(H11B), C2(H2), C1A(H1AD),
 C1A(H1AC), C10A(H10A), C14A(H14A), C11A(H11A), C4(H4)
5.b Aromatic/amide H refined with riding coordinates:
 C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A)
5.c Idealised Me refined as rotating group:
 C15B(H15A,H15B,H15C), C16B(H16A,H16B,H16C), C12B(H12A,H12B,H12C), C13B(H13A,
 H13B,H13C), C1(H1A,H1C,H1D), C3(H3A,H3B,H3C), C15A(H15D,H15E,H15F), C16A(H16D,
 H16E,H16F), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C5(H5C,H5D,H5E),
 C6(H6C,H6D,H6E)
;