Visible Light Mediated Photopolymerization in Single Crystals: Photomechanical Bending and Thermomechanical Unbending
Samanta, Ranita; Ghosh, Subhrokoli; Devarapalli, Ramesh; Reddy, C. Malla; Chemistry of Materials 30 (2018) 577–; doi:10.1021/acs.chemmater.7b04756

data_4002883
_publ_section_title
;
 Visible Light Mediated Photopolymerization in Single Crystals:
 Photomechanical Bending and Thermomechanical Unbending
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              577
_journal_paper_doi               10.1021/acs.chemmater.7b04756
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C42 H54 O6'
_chemical_formula_sum            'C42 H54 O6'
_chemical_formula_weight         654.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 116.10(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.916(4)
_cell_length_b                   4.8573(7)
_cell_length_c                   19.218(4)
_cell_measurement_reflns_used    2133
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      22.9920
_cell_measurement_theta_min      2.0790
_cell_volume                     1753.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -10.00 104.00   1.00    7.50    --   27.86  57.00-120.00  114
  2  \w     35.00 122.00   1.00    7.50    --   27.86 178.00-180.00   87
  3  \w    -28.00 110.00   1.00    7.50    --   27.86  38.00   0.00  138
  4  \w     -8.00  38.00   1.00    7.50    --  -23.50-112.00  -8.00   46
  5  \w     35.00 122.00   1.00    7.50    --   27.86 178.00  90.00   87
  6  \w     35.00 122.00   1.00    7.50    --   27.86 178.00   0.00   87
  7  \w    -54.00  83.00   1.00    7.50    --   27.86 -38.00 120.00  137
  8  \w    -59.00 112.00   1.00    7.50    --   27.86 -19.00-120.00  171
  9  \w    -10.00 104.00   1.00    7.50    --   27.86  57.00 120.00  114
 10  \w    -20.00  32.00   1.00    7.50    --  -23.50 -99.00  90.00   52
 11  \w    -20.00  32.00   1.00    7.50    --  -23.50 -99.00 -90.00   52
 12  \w    -20.00  32.00   1.00    7.50    --  -23.50 -99.00-120.00   52
 13  \w     35.00 122.00   1.00    7.50    --   27.86 178.00-150.00   87
 14  \w    -15.00 106.00   1.00    7.50    --   27.86  77.00 120.00  121
 15  \w    -10.00 104.00   1.00    7.50    --   27.86  57.00  30.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0292142000
_diffrn_orient_matrix_UB_12      -0.0228077000
_diffrn_orient_matrix_UB_13      -0.0086715000
_diffrn_orient_matrix_UB_21      0.0228378000
_diffrn_orient_matrix_UB_22      -0.0156010000
_diffrn_orient_matrix_UB_23      0.0400820000
_diffrn_orient_matrix_UB_31      -0.0071141000
_diffrn_orient_matrix_UB_32      -0.1433729000
_diffrn_orient_matrix_UB_33      -0.0029690000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1603
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23745
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             708
_exptl_crystal_preparation       'FORMED UNDER VISIBLE LIGHT'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0813
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+2.4189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                1860
_reflns_number_total             3099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm7b04756_si_005.cif
_cod_data_source_block           PBIT-dodeca2
_cod_depositor_comments          'Adding full bibliography for 4002883.cif.'
_cod_original_cell_volume        1753.5(5)
_cod_database_code               4002883
_chemical_oxdiff_formula         'C H O '
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.957
_oxdiff_exptl_absorpt_empirical_full_min 0.640