A new cyclic supramolecular Zn(ii) complex derived from a N2O2 oxime chelate ligand with luminescence mechanochromism.
Zhang, Shou-Ting; Li, Tian-Rong; Wang, Bao-Dui; Yang, Zheng-Yin; Liu, Jian; Wang, Zhi-Yi; Dong, Wen-Kui; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2713–2717; doi:10.1039/c3dt52340c

data_7028461
_publ_section_title
;
 A new cyclic supramolecular Zn(ii) complex derived from a N2O2 oxime
 chelate ligand with luminescence mechanochromism.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2713
_journal_page_last               2717
_journal_paper_doi               10.1039/c3dt52340c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C37 H34 N6 O5 Zn'
_chemical_formula_sum            'C37 H34 N6 O5 Zn'
_chemical_formula_weight         708.07
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-27
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                104.972(9)
_cell_angle_beta                 105.000(9)
_cell_angle_gamma                91.803(6)
_cell_formula_units_Z            2
_cell_length_a                   10.6014(8)
_cell_length_b                   10.6656(8)
_cell_length_c                   15.898(2)
_cell_measurement_reflns_used    5659
_cell_measurement_temperature    289.96(10)
_cell_measurement_theta_max      28.5666
_cell_measurement_theta_min      2.9584
_cell_volume                     1668.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      289.96(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.9786
_diffrn_measured_fraction_theta_max 0.9758
_diffrn_measurement_details
;
1 omega -8.00 89.00 1.0000 7.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 77.0000 0.0000 97

2 omega -11.00 16.00 1.0000 7.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 -57.0000 90.0000 27

3 omega -8.00 17.00 1.0000 7.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 77.0000 120.0000 25

4 omega -38.00 85.00 1.0000 7.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 19.0000 -60.0000 123

5 omega -99.00 -66.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- -19.3492 178.0000 -60.0000 33

6 omega -101.00 -76.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- -19.3492 178.0000 0.0000 25

7 omega 15.00 66.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 -99.0000 -150.0000 51

8 omega 71.00 97.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 -178.0000 30.0000 26

9 omega -48.00 13.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 -57.0000 -60.0000 61

10 omega 10.00 37.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 -99.0000 0.0000 27

11 omega 10.00 35.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 22.7867 57.0000 30.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0548580000
_diffrn_orient_matrix_UB_12      -0.0352072000
_diffrn_orient_matrix_UB_13      0.0042118000
_diffrn_orient_matrix_UB_21      -0.0074040000
_diffrn_orient_matrix_UB_22      0.0544882000
_diffrn_orient_matrix_UB_23      0.0345080000
_diffrn_orient_matrix_UB_31      -0.0422622000
_diffrn_orient_matrix_UB_32      0.0242084000
_diffrn_orient_matrix_UB_33      -0.0333942000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14909
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6683
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+0.5349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                5525
_reflns_number_total             6683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52340c.txt
_cod_data_source_block           zhangshouting0104
_cod_original_cell_volume        1668.0(3)
_cod_database_code               7028461
_reflns_odcompleteness_completeness 97.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H5A of C5, H4 of C4, H3 of C3, H2 of C2, H1 of C1, H13 of C13, H14 of C14,
H15 of C15, H16 of C16, H17 of C17, {H18A,H18B} of C18, {H19A,H19B} of C19,
H22 of C22, H23 of C23, H24 of C24, H25 of C25, H26 of C26, H32 of C32, H33
of C33, H34 of C34, H35 of C35, H36 of C36
At 1.5 times of:
H5 of O5, {H10A,H10B,H10C} of C10, {H29A,H29B,H29C} of C29, {H37A,H37B,
H37C} of C37A, {H37D,H37E,H37F} of C37B
2. Restrained distances
O5-H5
0.85 with sigma of 0.01
Zn1-H5
2.632472 with sigma of 0.02
C37A-H5
1.870328 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37A) ~ Ueq, Uanis(C37B) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) ~ Ueq, Uanis(C35) ~ Ueq, Uanis(C34) ~ Ueq, Uanis(C33) ~ Ueq, Uanis(C32) ~ Ueq, Uanis(C31)
~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
Fixed Sof: C37A(0.75) H37A(0.75) H37B(0.75) H37C(0.75) C37B(0.25) H37D(0.25)
H37E(0.25) H37F(0.25)
5.a Secondary CH2 refined with riding coordinates:
C18(H18A,H18B), C19(H19A,H19B)
5.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5A), C13(H13), C14(H14), C15(H15),
C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32),
C33(H33), C34(H34), C35(H35), C36(H36)
5.c Idealised Me refined as rotating group:
C10(H10A,H10B,H10C), C29(H29A,H29B,H29C), C37A(H37A,H37B,H37C), C37B(H37D,
H37E,H37F)
;