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_7041917
_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         'C35 H40 N4 O2'
_chemical_formula_sum            'C35 H40 N4 O2'
_chemical_formula_weight         548.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-10
_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                 98.3145(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9282(3)
_cell_length_b                   5.14524(8)
_cell_length_c                   19.5488(3)
_cell_measurement_reflns_used    12160
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.3920
_cell_measurement_theta_min      4.4960
_cell_volume                     1485.74(4)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -115.00  -12.10   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -46.0000  109.0000 147

  2 omega -115.00  -59.70   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680 -147.0000 -117.0000 79

  3 omega  -49.00   35.00   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680   37.0000  -90.0000 120

  4 omega -114.00  -10.40   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -57.0000    0.0000 148

  5 omega   57.00  128.40   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.0680  178.0000 -180.0000 102

  6 omega   72.00  177.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   77.0000  -90.0000 150

  7 omega   94.00  178.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  125.0000 -180.0000 120

  8 omega   73.00  176.60   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   70.0000  -29.5605 148

  9 omega   78.00  176.70   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   45.0000   60.0000 141

 10 omega   78.00  176.70   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   45.0000  -30.0000 141

 11 omega   72.00  177.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   77.0000  -30.0000 150

 12 omega   28.00   92.40   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -30.0000  -60.0000 92

 13 omega   72.00  177.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   77.0000  -60.0000 150

 14 omega   75.00  177.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   61.0000    0.0000 146

 15 omega   21.00  108.50   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  -94.0000  120.0000 125

 16 omega   75.00  177.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   61.0000   30.0000 146

 17 omega   94.00  178.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400  125.0000  150.0000 120

 18 omega   75.00  177.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   61.0000  -30.0000 146

 19 omega   78.00  176.70   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   45.0000 -150.0000 141

 20 omega   73.00  176.60   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   71.0000    6.3101 148

 21 omega   73.00  176.60   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   72.0000   -3.7799 148

 22 omega   75.00  177.20   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   30.0000    0.0000 146

 23 omega -119.00   -7.00   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -77.0000 -180.0000 160

 24 omega -114.00  -10.40   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -57.0000 -120.0000 148

 25 omega -119.00   -7.00   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.0680  -77.0000  -30.0000 160

 26 omega   57.00  128.40   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.0680  178.0000 -120.0000 102

 27 omega   55.00  127.10   0.7000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       40.0680 -178.0000   30.0000 103

 28 omega   31.00  121.30   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400 -125.0000  -30.0000 129

 29 omega   73.00  176.60   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   73.0000  110.9202 148

 30 omega   75.00  112.80   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   61.0000   90.0000 54

 31 omega   78.00  176.70   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   46.0000 -101.0000 141

 32 omega   72.00  177.00   0.7000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.5400   77.0000  150.0000 150
;
_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      0.0840759000
_diffrn_orient_matrix_UB_12      0.1679923000
_diffrn_orient_matrix_UB_13      -0.0053643000
_diffrn_orient_matrix_UB_21      -0.0256957000
_diffrn_orient_matrix_UB_22      0.0097022000
_diffrn_orient_matrix_UB_23      -0.0791648000
_diffrn_orient_matrix_UB_31      -0.0560639000
_diffrn_orient_matrix_UB_32      0.2478246000
_diffrn_orient_matrix_UB_33      0.0067346000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27124
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.624
_diffrn_reflns_theta_min         3.492
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36668
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.851
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2188 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     488
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.3490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                5387
_reflns_number_total             5829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04756d2.cif
_cod_data_source_block           str1740
_cod_depositor_comments
'Adding full bibliography for 7041914--7041918.cif.'
_cod_original_cell_volume        1485.75(4)
_cod_database_code               7041917
_chemical_oxdiff_formula         'C35 H40 N4 O2'
_reflns_odcompleteness_completeness 99.93
_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
2. Restrained distances
 C20A-C21A
 1.38 with sigma of 0.001
 N2-H2
 0.97 with sigma of 0.02
 C19-C18B
 1.38 with sigma of 0.001
 C18B-C17B
 1.38 with sigma of 0.001
 C17B-C16
 1.38 with sigma of 0.001
 C16-C21A
 1.38 with sigma of 0.001
 C21A-C20A
 1.38 with sigma of 0.001
 C20A-C19
 1.38 with sigma of 0.001
 C17A-C16
 1.38 with sigma of 0.001
 C24A-C23A
 1.38 with sigma of 0.001
 C25A-C24A
 1.38 with sigma of 0.001
 C26A-C25A
 1.38 with sigma of 0.001
 C26A-C27A
 1.38 with sigma of 0.001
 C28A-C27A
 1.38 with sigma of 0.001
 C28A-C23A
 1.38 with sigma of 0.001
 N1-H1
 0.97 with sigma of 0.02
 C21B-C20B
 1.38 with sigma of 0.001
 C19-C20B
 1.38 with sigma of 0.001
 N3-H3AA
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Sof(H19A)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=Sof(C21B)=Sof(H21B)=
 Sof(C20B)=Sof(H20B)=1-FVAR(1)
 Sof(H19)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C17A)=Sof(H17A)=
 Sof(C18A)=Sof(H18A)=FVAR(1)
 Sof(H3BB)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(C23B)=Sof(C24B)=Sof(H24B)=
 Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27B)=Sof(C28B)=
 Sof(H28B)=1-FVAR(2)
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=Sof(H26A)=Sof(C28A)=Sof(H28A)=
 Sof(H3AA)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C7(H7)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C15(H15A,H15B), C22B(H22A,
 H22B), C29(H29A,H29B), C22A(H22C,H22D)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C24B(H24B), C25B(H25B),
 C26B(H26B), C27B(H27B), C28B(H28B), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C19(H19), C19(H19A), C20A(H20A), C21A(H21A), C17B(H17B), C18B(H18B),
 C17A(H17A), C18A(H18A), C21B(H21B), C24A(H24A), C25A(H25A), C27A(H27A),
 C26A(H26A), C28A(H28A), C20B(H20B)
;