Photothermal Möbius aromatic metallapentalenofuran and its NIR-responsive copolymer
Lu, Zhengyu; Cai, Yuanting; Wei, Yuanqing; Lin, Qin; Chen, Jiangxi; He, Xumin; Li, Shunhua; Wu, Weitai; Xia, Haiping; Polymer Chemistry 9 (2018) 2092–; doi:10.1039/C8PY00176F

data_1549072
_publ_section_title
;
 Photothermal M\"obius aromatic metallapentalenofuran and its
 NIR-responsive copolymer
;
_journal_issue                   16
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2092
_journal_paper_doi               10.1039/C8PY00176F
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C73 H57 Cl O3 Os P3 S2, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C75 H61 B Cl5 F4 O3 Os P3 S2'
_chemical_formula_weight         1621.52
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-01-05 deposited with the CCDC.
2018-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7978(6)
_cell_length_b                   14.1129(3)
_cell_length_c                   20.1547(4)
_cell_measurement_reflns_used    64484
_cell_measurement_temperature    173
_cell_measurement_theta_max      55.03
_cell_measurement_theta_min      6.01
_cell_volume                     7006.1(3)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102445
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.003
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4674
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.379
_refine_diff_density_min         -2.720
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         16024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+7.0102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11750
_reflns_number_total             16024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00176f3.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1549072--1549073.cif.'
_cod_database_code               1549072
_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 Cl(H,H) groups
2. Shared sites
{C26', S2}
{S2', C26}
{C27', C28}
{C27, C28'}
3. Uiso/Uaniso restraints and constraints
Uanis(C26') = Uanis(S2)
Uanis(S2') = Uanis(C26)
Uanis(C27') = Uanis(C28)
Uanis(C27) = Uanis(C28')
Uanis(C2C) = Uanis(C3C) = Uanis(C4C) = Uanis(C5C) = Uanis(C6C) = Uanis(C1C)
4. Others
 Fixed Sof: Cl5(0.5) S2'(0.5) C28'(0.5) H28'(0.5) C27'(0.5) H27'(0.5)
 C26'(0.5) H26'(0.5) S2(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5)
 H28(0.5) Cl5A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C2H(H2H), C3(H3), C8(H8), C5(H5), C2D(H2D), C1(H1), C6G(H6G), C6F(H6F),
 C2A(H2A), C6E(H6E), C2B(H2B), C6D(H6D), C23(H23), C6B(H6B), C2F(H2F), C2I(H2I),
  C22(H22), C2G(H2G), C3A(H3A), C6I(H6I), C6A(H6A), C3H(H3H), C4G(H4G),
 C5G(H5G), C4A(H4A), C5F(H5F), C5E(H5E), C4F(H4F), C5I(H5I), C2E(H2E), C3F(H3F),
  C3I(H3I), C5B(H5B), C3G(H3G), C4I(H4I), C4E(H4E), C3E(H3E), C3D(H3D),
 C3B(H3B), C4H(H4H), C5A(H5A), C5D(H5D), C4B(H4B), C6H(H6H), C5H(H5H), C4D(H4D),
  C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C6C(H6C), C28'(H28'), C27'(H27'),
 C26'(H26'), C26(H26), C27(H27), C28(H28)
5.c Fitted hexagon refined as free rotating group:
 C2C(C3C,C4C,C5C,C6C,C1C)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              72704
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'