Facile redox state manipulation in Cu(i) frameworks by utilisation of the redox-active tris(4-(pyridin-4-yl)phenyl)amine ligand.
Hua, Carol; Turner, Peter; D'Alessandro, Deanna M; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15297–15303; doi:10.1039/c5dt01233c

data_1520103
_publ_section_title
;
 Facile redox state manipulation in Cu(i) frameworks by utilisation of the
 redox-active tris(4-(pyridin-4-yl)phenyl)amine ligand.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15297
_journal_page_last               15303
_journal_paper_doi               10.1039/c5dt01233c
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C34.5 H24 Cu N5.5 O5.62'
_chemical_formula_weight         669.13
_chemical_name_systematic        CuNPy3NO3
_space_group_crystal_system      orthorhombic
_space_group_IT_number           17
_space_group_name_Hall           'P 2c 2'
_space_group_name_H-M_alt        'P 2 2 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      17
_symmetry_space_group_name_Hall  'P 2c 2'
_symmetry_space_group_name_H-M   'P 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-03-24 deposited with the CCDC.
2015-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0770(16)
_cell_length_b                   13.831(2)
_cell_length_c                   32.773(6)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.33
_cell_volume                     4114.5(12)
_computing_cell_refinement       'SAINT (Bruker-AXS,2012)'
_computing_data_collection       'APEX (Bruker-AXS,2012)'
_computing_data_reduction        'SAINT and XPREP (Bruker-AXS,2012)'
_computing_molecular_graphics
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hbschle,C.B., et al., 2011) 
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       \w+\f
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            69365
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_min         1.472
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       balde
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         10282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.1071
_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^)+(0.2P)^2^+5.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3008
_refine_ls_wR_factor_ref         0.3179
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8019
_reflns_number_total             10282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01233c2.cif
_cod_data_source_block           CuNPy3NO3_sx_oP
_cod_depositor_comments
'Adding full bibliography for 1520101--1520104.cif.'
_cod_original_cell_volume        4114.4(12)
_cod_original_formula_sum        'C34.50 H24 Cu N5.50 O5.62'
_cod_database_code               1520103
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              79843