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_1549073
_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         'C77 H59 Cl O3 Os P3 S3, B F4'
_chemical_formula_sum            'C77 H59 B Cl F4 O3 Os P3 S3'
_chemical_formula_weight         1533.79
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_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                76.6530(10)
_cell_angle_beta                 84.0290(10)
_cell_angle_gamma                69.3370(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1803(3)
_cell_length_b                   14.1709(4)
_cell_length_c                   23.4379(6)
_cell_measurement_reflns_used    37295
_cell_measurement_temperature    173
_cell_measurement_theta_max      55.07
_cell_measurement_theta_min      6.02
_cell_volume                     3379.62(16)
_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  0.0842
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54869
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.008
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.567
_refine_diff_density_min         -2.818
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         15481
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1074P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11933
_reflns_number_total             15481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00176f3.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 1549072--1549073.cif.'
_cod_database_code               1549073
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(B1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C122(H122), C126(H126), C326(H326), C136(H136), C322(H322),
 C212(H212), C232(H232), C336(H336), C112(H112), C3(H3), C216(H216), C316(H316),
  C312(H312), C226(H226), C116(H116), C5(H5), C113(H113), C132(H132),
 C125(H125), C133(H133), C236(H236), C124(H124), C23(H23), C323(H323),
 C225(H225), C114(H114), C224(H224), C213(H213), C233(H233), C234(H234),
 C325(H325), C332(H332), C22(H22), C314(H314), C313(H313), C235(H235),
 C115(H115), C134(H134), C315(H315), C135(H135), C214(H214), C123(H123),
 C324(H324), C215(H215), C335(H335), C222(H222), C223(H223), C333(H333),
 C334(H334), C26(H26), C27(H27), C32(H32), C30(H30), C31(H31)
3.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              18055
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'