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_4348170
_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 Ni O2, H2 O'
_chemical_formula_sum            'C16 H26 N4 Ni O3'
_chemical_formula_weight         381.11
_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            8
_cell_length_a                   11.1735(3)
_cell_length_b                   15.6927(4)
_cell_length_c                   21.4976(5)
_cell_measurement_reflns_used    19836
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      28.9840
_cell_measurement_theta_min      3.1700
_cell_volume                     3769.44(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
  1 omega  -83.00   15.00   0.4000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -38.0000   90.0000 245

  2 omega  -63.00  -37.00   0.4000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  130.0000    8.1429 65

  3 omega   17.00   43.00   0.4000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -99.0000  -90.0000 65

  4 omega  -27.00   41.00   0.4000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -77.0000  -60.0000 170

  5 omega  -38.00   62.00   0.4000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   38.0000  120.0000 250

  6 omega  -14.00   88.00   0.4000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191   38.0000   60.0000 255
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0047680000
_diffrn_orient_matrix_UB_12      -0.0027665000
_diffrn_orient_matrix_UB_13      0.0328592000
_diffrn_orient_matrix_UB_21      0.0264346000
_diffrn_orient_matrix_UB_22      0.0410338000
_diffrn_orient_matrix_UB_23      0.0008605000
_diffrn_orient_matrix_UB_31      -0.0575882000
_diffrn_orient_matrix_UB_32      0.0185882000
_diffrn_orient_matrix_UB_33      0.0030570000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41812
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.451
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43351
_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    1.343
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3472 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0376P)^2^+0.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                8785
_reflns_number_total             9424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01066_si_002.cif
_cod_data_source_block           9c-str1589
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H52 N8 Ni2 O6'
_cod_original_formula_weight         762.23
_cod_original_formula_moiety         '2(C16 H24 N4 Ni O2), 2(H2 O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        3769.44(17)
_cod_database_code               4348170
_chemical_oxdiff_formula         'C16 H20 O2 N4 Ni'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H2A-O2 = O2-H2B
 0.85 with sigma of 0.02
 H2A-H2B
 1.367 with sigma of 0.04
3.a Free rotating group:
 O1(H1C,H1D)
3.b Ternary CH refined with riding coordinates:
 C1B(H1B), C10B(H10B), C11B(H11B), C14B(H14B), C1A(H1A), C10A(H10A),
 C11A(H11A), C14A(H14A)
3.c Secondary CH2 refined with riding coordinates:
 N1B(H1BA,H1BB), N2B(H2BA,H2BB), N1A(H1AA,H1AB), N2A(H2AA,H2AB)
3.d Aromatic/amide H refined with riding coordinates:
 C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A)
3.e Idealised Me refined as rotating group:
 C12B(H12A,H12B,H12C), C13B(H13A,H13B,H13C), C15B(H15A,H15B,H15C), C16B(H16A,
 H16B,H16C), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F),
 C16A(H16D,H16E,H16F)
;