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_7041914
_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 Cu N4 O2, 2(H2 O)'
_chemical_formula_sum            'C35 H42 Cu N4 O4'
_chemical_formula_weight         646.26
_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                 97.225(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6591(3)
_cell_length_b                   15.9975(4)
_cell_length_c                   10.4363(3)
_cell_measurement_reflns_used    12926
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5940
_cell_measurement_theta_min      3.2100
_cell_volume                     1599.83(8)
_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      297.9(6)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30342
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.993
_exptl_absorpt_coefficient_mu    0.727
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 2592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6280
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.602
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0555P)^2^+0.1541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5864
_reflns_number_total             6280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04756d2.cif
_cod_data_source_block           str1605
_cod_depositor_comments
'Adding full bibliography for 7041914--7041918.cif.'
_cod_original_cell_volume        1599.82(8)
_cod_database_code               7041914
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 H3D-O3 = O3-H3C
 0.85 with sigma of 0.00001
 H4C-O4 = O4-H4D
 0.85 with sigma of 0.00001
 H3D-H3C
 1.367 with sigma of 0.00002
 H4C-H4D
 1.367 with sigma of 0.00002
3.a Free rotating group:
 O4(C17,C16,C29,C5,C21,C15,C3,C4,O2,C20,C18,C19,O3,H3C,H3D,H4C,H4D)
3.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C7(H7)
3.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C22(H22A,H22B), C29(H29A,H29B), C5(H5A,H5B), C15(H15A,H15B),
 C3(H3A,H3B), C4(H4A,H4B)
3.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C17(H17), C21(H21), C20(H20), C18(H18), C19(H19)
3.e Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C13,C14), C23(C24,C25,C26,C27,C28), C30(C31,C32,C33,C34,C35)
;