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_7041915
_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 N4 Ni O2, H2 O'
_chemical_formula_sum            'C27 H40 N4 Ni O3'
_chemical_formula_weight         527.34
_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                   11.0695(3)
_cell_length_b                   15.2253(4)
_cell_length_c                   16.1040(5)
_cell_measurement_reflns_used    11185
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      28.1780
_cell_measurement_theta_min      3.4720
_cell_volume                     2714.11(13)
_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      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega  -19.00   10.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877  -99.0000   90.0000 29

  2 omega  -32.00   66.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877   38.0000  -30.0000 98

  3 omega  -11.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   38.0000   60.0000 70

  4 omega -106.00  -57.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5877 -178.0000  -30.0000 49

  5 omega  -17.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   38.0000  -90.0000 111

  6 omega  -21.00   28.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   77.0000    0.0000 49

  7 omega  -20.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -99.0000 -150.0000 79
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0569725000
_diffrn_orient_matrix_UB_12      -0.0212185000
_diffrn_orient_matrix_UB_13      -0.0024761000
_diffrn_orient_matrix_UB_21      -0.0260940000
_diffrn_orient_matrix_UB_22      0.0337620000
_diffrn_orient_matrix_UB_23      0.0244083000
_diffrn_orient_matrix_UB_31      -0.0135970000
_diffrn_orient_matrix_UB_32      0.0240679000
_diffrn_orient_matrix_UB_33      -0.0365542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_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       -21
_diffrn_reflns_number            30689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.279
_diffrn_reflns_theta_min         2.862
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47998
_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    1.291
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.2208
_exptl_crystal_size_mid          0.1231
_exptl_crystal_size_min          0.0868
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 2281 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6801
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0414P)^2^+0.9621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                5903
_reflns_number_total             6801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04756d2.cif
_cod_data_source_block           str1580
_cod_depositor_comments
'Adding full bibliography for 7041914--7041918.cif.'
_cod_database_code               7041915
_chemical_oxdiff_formula         'C28 H36 N2 O2 Ni'
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1 = N4-H4
 0.97 with sigma of 0.02
3.a Free rotating group:
 O3(H3C,H3D)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C17(H17), C18(H18)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C1(H1A,H1B), C21(H21A,H21B), C3(H3A,H3B)
3.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C11(H11), C26(H26), C23(H23), C24(H24), C27(H27),
 C13(H13), C14(H14), C25(H25)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;