Pillar-template strategy switching the redox activity and magnetic properties of trisphenylamine-based coordination polymers
Qiu, Ya-Ru; Li, Bang; Zhou, Yan; Su, Jian; Ge, Jing-Yuan; CrystEngComm  (2020) –; doi:10.1039/D0CE00256A

data_7240157
_publ_section_title
;
 Pillar-template strategy switching the redox activity and magnetic
 properties of trisphenylamine-based coordination polymers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00256A
_journal_year                    2020
_chemical_formula_moiety         'C33 H24 N6 Ni O6'
_chemical_formula_sum            'C33 H24 N6 Ni O6'
_chemical_formula_weight         659.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.807(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.683(3)
_cell_length_b                   15.164(3)
_cell_length_c                   19.852(3)
_cell_measurement_reflns_used    5605
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.6
_cell_volume                     6365.0(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5605
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.8010
_exptl_absorpt_correction_T_min  0.7773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5605
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+8.4026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                4291
_reflns_number_total             5605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce00256a2.cif
_cod_data_source_block           2-Ni
_cod_original_cell_volume        6365.2(18)
_cod_database_code               7240157
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 O5, N6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Ni1 \\sim N5 \\sim O1 \\sim O2 \\sim O3: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O3) = Uanis(O3')
Uanis(O2) = Uanis(O2')
Uanis(O1) = Uanis(O1')
Uanis(N5) = Uanis(N5')
4. Others
 Sof(N5')=Sof(O1')=Sof(O2')=Sof(O3')=1-FVAR(1)
 Sof(N5)=Sof(O1)=Sof(O2)=Sof(O3)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33)
;
_olex2_submission_special_instructions 'No special instructions were received'