Features of styryl dye crystal packings and their influence on [2 + 2] photocycloaddition reaction with single crystal retention
Kuz'mina, Lyudmila G.; Vedernikov, Artem I.; Howard, Judith A. K.; Alfimov, Michael V.; Gromov, Sergey P.; CrystEngComm 17 (2015) 4584–; doi:10.1039/C5CE00653H

data_7220484
_publ_section_title
;
 Features of styryl dye crystal packings and their influence on [2 + 2]
 photocycloaddition reaction with single crystal retention
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4584
_journal_paper_doi               10.1039/C5CE00653H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'I, C20 H22 N O3 S, 0.5(O)'
_chemical_formula_sum            'C20 H22 I N O3.5 S'
_chemical_formula_weight         491.37
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                110.533(2)
_cell_angle_beta                 91.966(2)
_cell_angle_gamma                94.712(2)
_cell_formula_units_Z            4
_cell_length_a                   7.4692(4)
_cell_length_b                   15.9898(9)
_cell_length_c                   18.4114(11)
_cell_measurement_reflns_used    9899
_cell_measurement_theta_max      30.585
_cell_measurement_theta_min      2.368
_cell_volume                     2047.5(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.9828
_diffrn_measured_fraction_theta_max 0.9845
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31145
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5939
_exptl_crystal_description       prism
_exptl_crystal_F_000             983.2515
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.1516
_refine_diff_density_min         -0.8272
_refine_diff_density_rms         0.3028
_refine_ls_d_res_high            0.7330
_refine_ls_d_res_low             8.9506
_refine_ls_goodness_of_fit_ref   1.0103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    70
_refine_ls_number_parameters     485
_refine_ls_number_reflns         10716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0103
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1090P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              20
_reflns_limit_k_min              -21
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                9654
_reflns_number_total             10716
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5ce00653h1.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7220483--7220487.cif.'
_cod_database_code               7220484
_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
2.a Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C19A(H19c,H19d)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C9(H9), C14(H14), C16(H16), C17(H17),
 C2A(H2A), C3A(H3A), C5A(H5A), C8A(H8A), C9A(H9A), C14A(H14A), C16A(H16A),
 C17A(H17A)
2.c Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C18(H18a,H18b,H18c), C20(H20a,H20b,
 H20c), C10A(H10d,H10e,H10f), C11A(H11d,H11e,H11f), C18A(H18d,H18e,H18f),
 C20A(H20d,H20e,H20f)
;
_olex2_submission_special_instructions 'No special instructions were received'