Magnetic and luminescent binuclear double-stranded helicates.
Cucos, Paula; Tuna, Floriana; Sorace, Lorenzo; Matei, Iulia; Maxim, Catalin; Shova, Sergiu; Gheorghe, Ruxandra; Caneschi, Andrea; Hillebrand, Mihaela; Andruh, Marius; Inorganic chemistry 53 (2014) 7738–7747; doi:10.1021/ic501051q

data_4340357
_publ_section_title
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 Magnetic and luminescent binuclear double-stranded helicates.
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_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7738
_journal_page_last               7747
_journal_paper_doi               10.1021/ic501051q
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C28 H22 Cu N2 O5, 0.5(C3 H7 N O), 0.2(H2 O)'
_chemical_formula_sum            'C29.5 H25.9 Cu N2.5 O5.7'
_chemical_formula_weight         570.17
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-24
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:32:32, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.2756(7)
_cell_length_b                   14.2756(7)
_cell_length_c                   27.1417(14)
_cell_measurement_reflns_used    2533
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9942
_cell_measurement_theta_min      2.5097
_cell_volume                     5531.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -43.00  -17.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8565  -57.0000  120.0000 26

  2 omega  -46.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6690  -57.0000 -150.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0359591000
_diffrn_orient_matrix_UB_12      -0.0005954000
_diffrn_orient_matrix_UB_13      -0.0180312000
_diffrn_orient_matrix_UB_21      0.0216079000
_diffrn_orient_matrix_UB_22      0.0389808000
_diffrn_orient_matrix_UB_23      0.0115564000
_diffrn_orient_matrix_UB_31      0.0266084000
_diffrn_orient_matrix_UB_32      -0.0308088000
_diffrn_orient_matrix_UB_33      0.0149822000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            11728
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5428
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2193
_reflns_number_gt                3512
_reflns_number_total             5428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501051q_si_002.cif
_cod_data_source_block           shi_892_maan
_cod_depositor_comments
'Adding full bibliography for 4340357--4340359.cif.'
_cod_original_formula_sum        'C29.50 H25.90 Cu N2.50 O5.70'
_cod_database_code               4340357
_chemical_oxdiff_formula         'C20 H30 N4 O4 Cu1 Cd1'
_chemical_oxdiff_usercomment     AI_3
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H29 of C29, H4 of C4, H21 of C21, H13 of C13, H18 of C18, H19 of C19, H7 of
  C7, H12 of C12, H11 of C11, H28 of C28, H3 of C3, H5 of C5, H25 of C25, H24
  of C24, H27 of C27, H9 of C9, H22 of C22
 At 1.5 times of:
  {H1WA,H1WB} of O1W, {H30A,H30B,H30C} of C30, {H31A,H31B,H31C} of C31, {H8A,
  H8B,H8C} of C8, {H16A,H16B,H16C} of C16
2. Restrained distances
 N3-C29
 1.4 with sigma of 0.02
 O6-C29
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(N3) = Uiso(C31) = Uiso(O6) = Uiso(C30) = Uiso(C29)
4. Others
 Fixed Sof: N3(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) O6(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) C29(0.5) H29(0.5) O1W(0.2) H1WA(0.2) H1WB(0.2)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C19(H19), C7(H7), C9(H9), C22(H22), C27(H27), C24(H24),
 C25(H25), C5(H5), C3(H3), C28(H28), C11(H11), C12(H12), C4(H4), C29(H29)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C)
;