Cu(2+) recognition by N,N'-benzylated bis(amino amides).
Gorla, Lingaraju; Martí-Centelles, Vicente; Altava, Belén; Burguete, M. Isabel; Luis, Santiago V.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2660–2669; doi:10.1039/c6dt04756d

data_7041918
_publ_section_title
;
 Cu(2+) recognition by N,N'-benzylated bis(amino amides).
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2660
_journal_page_last               2669
_journal_paper_doi               10.1039/c6dt04756d
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C27 H38 Cu N4 O2, H2 O'
_chemical_formula_sum            'C27 H40 Cu N4 O3'
_chemical_formula_weight         532.17
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-05-20 deposited with the CCDC.
2017-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8225(2)
_cell_length_b                   15.3302(3)
_cell_length_c                   16.2148(3)
_cell_measurement_reflns_used    14314
_cell_measurement_temperature    141(20)
_cell_measurement_theta_max      28.6480
_cell_measurement_theta_min      3.6500
_cell_volume                     2690.22(9)
_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)'
_diffrn_ambient_temperature      141(20)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
  1 omega  -20.00    5.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603  -99.0000 -120.0000 25

  2 omega  -32.00   -6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603   77.0000  -90.0000 26

  3 omega  -20.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8322   57.0000  -60.0000 111

  4 omega   15.00   72.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8322   38.0000   30.0000 57

  5 omega -110.00  -55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603  178.0000   60.0000 55

  6 omega  -20.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8322   38.0000   90.0000 105

  7 omega  -68.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.8322  -38.0000  -60.0000 122
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0074395000
_diffrn_orient_matrix_UB_12      -0.0457336000
_diffrn_orient_matrix_UB_13      0.0044021000
_diffrn_orient_matrix_UB_21      -0.0650705000
_diffrn_orient_matrix_UB_22      -0.0050442000
_diffrn_orient_matrix_UB_23      0.0021627000
_diffrn_orient_matrix_UB_31      -0.0024675000
_diffrn_orient_matrix_UB_32      -0.0048858000
_diffrn_orient_matrix_UB_33      -0.0434657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29728
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.095
_diffrn_reflns_theta_min         2.842
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71128
_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_density_diffrn    1.314
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2381 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6665
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0219P)^2^+0.9116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                6101
_reflns_number_total             6665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04756d2.cif
_cod_data_source_block           str1570
_cod_depositor_comments
'Adding full bibliography for 7041914--7041918.cif.'
_cod_database_code               7041918
_chemical_oxdiff_formula         'C27 H40 N4 O2 Cu'
_reflns_odcompleteness_completeness 99.71
_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 C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-H3A
 0.9 with sigma of 0.02
 O3-H3B
 0.9 with sigma of 0.02
3. Others
 Sof(H3BC)=Sof(H3BD)=Sof(H5BC)=Sof(H5BD)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(H5AA)=Sof(H5AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C7(H7), C8(H8), C11(H11)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C5(H5AA,H5AB), C5(H5BC,H5BD), C14(H14A,H14B),
 C21(H21A,H21B), C4A(H4AA,H4AB), C4B(H4BA,H4BB)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;