Amphipathic Metal-Containing Macromolecules with Photothermal Properties
He, Xumin; He, Xiehua; Li, Shenyan; Zhuo, Kaiyue; Qin, Weixiang; Dong, Shuyu; Chen, Jiangxi; Ren, Lei; Liu, Gang; Xia, Haiping; Polym. Chem.  (2017) –; doi:10.1039/C7PY00641A

data_1546068
_publ_section_title
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 Amphipathic Metal-Containing Macromolecules with Photothermal Properties
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_journal_name_full               'Polym. Chem.'
_journal_paper_doi               10.1039/C7PY00641A
_journal_year                    2017
_chemical_formula_moiety         'C82 H64 O Os P3, C24 H20 B, 3(C H2 Cl2)'
_chemical_formula_sum            'C109 H90 B Cl6 O Os P3'
_chemical_formula_weight         1922.42
_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
_audit_creation_date             2015-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
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2017-03-03 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
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_cell_angle_alpha                79.946(3)
_cell_angle_beta                 89.601(3)
_cell_angle_gamma                82.370(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8163(5)
_cell_length_b                   18.0472(5)
_cell_length_c                   18.3229(6)
_cell_measurement_reflns_used    41288
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.145
_cell_measurement_theta_min      3.185
_cell_volume                     4458.1(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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41288
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        62.145
_diffrn_reflns_theta_max         62.145
_diffrn_reflns_theta_min         3.185
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70159
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         13981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+3.9212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12853
_reflns_number_total             13981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py00641a2.cif
_cod_data_source_block           hxh150402-2
_cod_original_cell_volume        4458.2(2)
_cod_database_code               1546068
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C3B(0.4) H3BA(0.4) H3BB(0.4) H3BC(0.4) Cl1(0.65) Cl4(0.65)
 C5BA(0.65) H5BA(0.65) H5BB(0.65) Cl2A(0.75) H4BA(0.75) H4BB(0.75) H4BC(0.25)
 H4BD(0.25) Cl2(0.35) Cl3(0.35) C5CA(0.35) H5CA(0.35) H5CB(0.35) Cl5(0.25)
 C15(0.6) H15A(0.6) H15B(0.6) H15C(0.6)
3.a Ternary CH refined with riding coordinates:
 C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C4CA(H4CA,H4CB), C5BA(H5BA,H5BB), C4BA(H4BA,H4BB), C4BA(H4BC,H4BD), C5CA(H5CA,
 H5CB)
3.c Aromatic/amide H refined with riding coordinates:
 C2BA(H2BA), C8(H8), C0AA(H0AA), C2AA(H2AA), C4AA(H4AA), C6(H6), C10(H10),
 C9BA(H9BA), C0CA(H0CA), C1(H1), C8AA(H8AA), C9AA(H9AA), C32(H32), C5(H5),
 C38(H38), C3(H3), C2CA(H2CA), C43(H43), C45(H45), C47(H47), C9CA(H9CA),
 C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C58(H58), C60(H60), C61(H61),
  C62(H62), C64(H64), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71),
 C72(H72), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82),
  C83(H83), C85(H85), C86(H86), C87(H87), C90(H90), C91(H91), C92(H92),
 C95(H95), C96(H96), C97(H97), C99(H99), C100(H100), C1BA(H1BA), C8BA(H8BA),
 C5AA(H5AA), C3CA(H3CA), C6CA(H6CA), C7CA(H7CA), C8CA(H8CA), C1DA(H1DA),
 C2DA(H2DA), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28),
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C0BA(H0BA),
 C7AA(H7AA)
3.d Idealised Me refined as rotating group:
 C3B(H3BA,H3BB,H3BC), C15(H15A,H15B,H15C)
3.e :
 C17(H17)
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_shelx_res_checksum              50492
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'