Selective complexation of di-n-hexylammonium salts by tailed porphyrin host
Liu, Hui; Tu, Ji-Qiang; Zhang, Cheng-Hua; Xiao, Qiao-Ting; Wang, Tian-Hua; Ju, Xiu-Lian; New J. Chem. 40 (2016) 5679–; doi:10.1039/C6NJ00045B

data_7055595
_publ_section_title
;
 Selective complexation of di-n-hexylammonium salts by tailed porphyrin
 host
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5679
_journal_paper_doi               10.1039/C6NJ00045B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C48 H37 N5 O2 Zn'
_chemical_formula_sum            'C48 H37 N5 O2 Zn'
_chemical_formula_weight         781.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-17 deposited with the CCDC.
2016-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.498(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.412(4)
_cell_length_b                   15.341(6)
_cell_length_c                   24.640(9)
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.37
_cell_measurement_theta_min      2.26
_cell_volume                     4212(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20500
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        21.675
_diffrn_reflns_theta_max         21.675
_diffrn_reflns_theta_min         1.693
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1176 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.8091.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
The disordered solvent molecules cannot be modeled and were treated 
by PLATON,SQUEEZE,1998.
There are total 90e per unit cell were accumulated which corresponds 
to 22.5e per formula. The 22.5e might come from one methanol molecule and were not included in the formula.
;
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         4879
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3330
_reflns_number_total             4879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00045b2.cif
_cod_data_source_block           1445583
_cod_depositor_comments          'Adding full bibliography for 7055595.cif.'
_cod_database_code               7055595
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained planarity
 C21A, C22A, C23A, C24A, C25A, C26A
 with sigma of 0.01
 C21, C22, C23, C24, C25, C26
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 O1, C45, C46, O2, C47, C48, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 O1A, C45A, C46A, O2A, C47A, C48A, N5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C21A, C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Others
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(1)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(1)
 Sof(N5A)=Sof(H5AA)=Sof(H5AB)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C47A)=
 Sof(H47C)=Sof(H47D)=Sof(O2A)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C45A)=Sof(H45C)=
 Sof(H45D)=Sof(O1A)=1-FVAR(2)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=
 Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(N5)=Sof(H5A)=Sof(H5B)=Sof(O1)=
 Sof(O2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), N5(H5A,H5B),
 N5A(H5AA,H5AB), C48A(H48C,H48D), C47A(H47C,H47D), C46A(H46C,H46D), C45A(H45C,
 H45D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1AA(H1AA), C7(H7), C2AA(H2AA), C12(H12), C13(H13), C17(H17),
 C18(H18), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C22A(H22A), C23A(H23A),
 C24A(H24A), C25A(H25A), C26A(H26A)
;
_shelx_res_checksum              15567
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'