Influence of the anion nature on styryl dye crystal packing and feasibility of the direct and back [2 + 2] photocycloaddition reactions without single crystal degradation
Kuz'mina, Lyudmila G.; Vedernikov, Artem I.; Churakov, Andrei V.; Lermontova, Elmira Kh.; Howard, Judith A. K.; Alfimov, Michael V.; Gromov, Sergey P.; CrystEngComm 16 (2014) 5364–; doi:10.1039/c4ce00266k

data_7215801
_publ_section_title
;
 Influence of the anion nature on styryl dye crystal packing and
 feasibility of the direct and back [2 + 2] photocycloaddition reactions
 without single crystal degradation
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              5364
_journal_paper_doi               10.1039/c4ce00266k
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'2(C7 H7 O3 S), 2(C17 H20 N O2), 2(H2 O), O, C2 H3 N'
_chemical_formula_sum            'C50 H63 N3 O13 S2'
_chemical_formula_weight         978.15
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.2560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6904(6)
_cell_length_b                   21.8223(8)
_cell_length_c                   15.8024(6)
_cell_measurement_temperature    120.0(2)
_cell_volume                     4971.1(3)
_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      120.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1608
_diffrn_reflns_av_unetI/netI     0.2023
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39135
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9243
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         11991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.2219
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.189
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1891
_reflns_number_gt                4480
_reflns_number_total             11991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00266k1.cif
_cod_data_source_block           tt
_cod_depositor_comments
'Adding full bibliography for 7215801--7215808.cif.'
_cod_database_code               7215801
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O4W)=Sof(H4WA)=Sof(H4WB)=1-FVAR(1)
 Sof(O3W)=Sof(H3WA)=Sof(H3WB)=FVAR(1)
3.a Free rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C16'(H16C,H16D)
3.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C2A'(H2A'), C3A'(H3A'), C5A'(H5A'),
 C6A'(H6A'), C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10),
 C13(H13), C1'(H1'), C2'(H2'), C4'(H4'), C5'(H5'), C6'(H6'), C7'(H7'), C9'(H9'),
  C10'(H10'), C13'(H13')
3.d Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7A'(H7AD,H7AE,H7AF), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C14'(H14D,H14E,H14F), C15'(H15D,H15E,H15F),
 C17'(H17D,H17E,H17F), C2S(H2SA,H2SB,H2SC)
;