Phenylamino derivatives of tris(2-pyridylmethyl)amine: hydrogen-bonded peroxodicopper complexes
Dahl, E. W.; Dong, H. T.; Szymczak, N. K.; Chemical Communications  (2018) –; doi:10.1039/C7CC08619A

data_7121006
_publ_section_title
;
 Phenylamino derivatives of tris(2-pyridylmethyl)amine: hydrogen-bonded
 peroxodicopper complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC08619A
_journal_year                    2018
_chemical_formula_moiety         'C36 H33 Cu N7 O, 2(C H2 Cl2), B C24 F20'
_chemical_formula_sum            'C62 H37 B Cl4 Cu F20 N7 O'
_chemical_formula_weight         1492.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-30
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-07 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                106.175(5)
_cell_angle_beta                 102.188(5)
_cell_angle_gamma                107.466(6)
_cell_formula_units_Z            2
_cell_length_a                   13.7619(9)
_cell_length_b                   14.9539(9)
_cell_length_c                   16.6243(7)
_cell_measurement_reflns_used    10451
_cell_measurement_temperature    85
_cell_measurement_theta_max      67.2050
_cell_measurement_theta_min      2.9050
_cell_volume                     2967.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      85
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43076
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.832
_diffrn_reflns_theta_min         2.923
_exptl_absorpt_coefficient_mu    3.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         10724
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1727P)^2^+1.2716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2417
_refine_ls_wR_factor_ref         0.2918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7688
_reflns_number_total             10724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08619a2.cif
_cod_data_source_block           2H
_cod_original_cell_volume        2967.6(3)
_cod_database_code               7121006
_shelx_shelxl_version_number     2016/6
_oxdiff_exptl_absorpt_empirical_full_min 0.394
_oxdiff_exptl_absorpt_empirical_full_max 2.729
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N5-H5 \\sim N6-H6 \\sim N7-H7
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C13(H13A,H13B), C61(H61A,H61B), C62(H62A,H62B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5A), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              78045
_olex2_submission_special_instructions 'No special instructions were received'