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_7041916
_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 H38 N4 Ni O2, 2(H2 O)'
_chemical_formula_sum            'C35 H42 N4 Ni O4'
_chemical_formula_weight         641.43
_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             2015-11-21
_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                   10.35136(10)
_cell_length_b                   15.75766(13)
_cell_length_c                   19.30342(19)
_cell_measurement_reflns_used    15352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.2010
_cell_measurement_theta_min      3.6050
_cell_volume                     3148.64(5)
_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)'
_diffrn_ambient_temperature      150.0
_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 0.994
_diffrn_measurement_details
;
  1 omega  -49.00   41.40   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   37.0000  -90.0000 113

  2 omega  -49.00   41.40   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   37.0000    0.0000 113

  3 omega   64.00  128.00   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  170.0000   59.0000 80

  4 omega  -42.00   68.40   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       37.6057  -37.0000 -180.0000 138

  5 omega   26.00   90.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -30.0000    0.0000 80

  6 omega  100.00  177.60   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  114.0000    8.0000 97

  7 omega   26.00   90.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -30.0000 -120.0000 80

  8 omega   20.00  108.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -94.0000  -60.0000 110

  9 omega   29.00   97.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -45.0000 -180.0000 85

 10 omega   26.00   90.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -30.0000   60.0000 80

 11 omega   20.00  108.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -94.0000 -150.0000 110

 12 omega   26.00   90.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -30.0000  -60.0000 80

 13 omega -116.00   -5.60   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000  120.0000 138

 14 omega -116.00   -5.60   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000    0.0000 138

 15 omega -116.00   -5.60   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -57.0000 -120.0000 138

 16 omega   69.00  177.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774   30.0000  -90.0000 135

 17 omega   43.00  177.40   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774   18.0000 -177.0000 168

 18 omega   20.00  108.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774  -94.0000   60.0000 110

 19 omega   74.00  126.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774   61.0000   60.0000 65

 20 omega   69.00  177.00   0.8000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3774   30.0000    0.0000 135
;
_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      0.0072881000
_diffrn_orient_matrix_UB_12      0.0603668000
_diffrn_orient_matrix_UB_13      -0.0626548000
_diffrn_orient_matrix_UB_21      -0.0349801000
_diffrn_orient_matrix_UB_22      0.0753708000
_diffrn_orient_matrix_UB_23      0.0472378000
_diffrn_orient_matrix_UB_31      0.1444670000
_diffrn_orient_matrix_UB_32      0.0152265000
_diffrn_orient_matrix_UB_33      0.0146206000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29035
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.129
_diffrn_reflns_theta_min         3.621
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.892
_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    1.353
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.3663
_exptl_crystal_size_mid          0.1019
_exptl_crystal_size_min          0.0671
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2423 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0694P)^2^+0.9703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                5759
_reflns_number_total             6132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04756d2.cif
_cod_data_source_block           str1646
_cod_depositor_comments
'Adding full bibliography for 7041914--7041918.cif.'
_cod_database_code               7041916
_chemical_oxdiff_formula         'C35 H40 N4 O2 Ni'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-H1 = N4-H4
 0.97 with sigma of 0.02
 H4A-O4 = O4-H4B
 0.85 with sigma of 0.02
 H3D-O3 = O3-H3C
 0.85 with sigma of 0.02
 H4A-H4B
 1.367 with sigma of 0.04
 H3D-H3C
 1.367 with sigma of 0.04
3.a Ternary CH refined with riding coordinates:
 C21(H21), C5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C1(H1A,H1B), C22(H22A,H22B), C6(H6A,H6B), C29(H29A,
 H29B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C26(H26), C25(H25), C24(H24), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C35(H35), C34(H34), C33(H33), C32(H32), C31(H31), C15(H15),
  C16(H16), C17(H17), C18(H18), C19(H19)
;