Turning over on sticky balls: preparation and catalytic studies of surface-functionalized TiO2 nanoparticles
Freimann, Sven A.; Prescimone, Alessandro; Housecroft, Catherine E.; Constable, Edwin C.; RSC Advances 11 (2021) 5537–5547; doi:10.1039/D0RA09319J

data_7242203
_publ_section_title
;
 Turning over on sticky balls: preparation and catalytic studies of
 surface-functionalized TiO2 nanoparticles
;
_journal_issue                   10
_journal_name_full               'RSC Advances'
_journal_page_first              5537
_journal_page_last               5547
_journal_paper_doi               10.1039/D0RA09319J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C50 H48 N6 O6 P2 Rh, 3(F6 P), C2 H3 N'
_chemical_formula_sum            'C52 H51 F18 N7 O6 P5 Rh'
_chemical_formula_weight         1469.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-27 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                73.903(4)
_cell_angle_beta                 83.442(4)
_cell_angle_gamma                82.315(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2477(7)
_cell_length_b                   14.0636(8)
_cell_length_c                   19.8182(11)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.132
_cell_measurement_theta_min      3.489
_cell_volume                     3239.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37630
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.543
_diffrn_reflns_theta_min         3.289
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.223
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.7673.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.824
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         11469
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.1061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1763P)^2^+18.1836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2968
_refine_ls_wR_factor_ref         0.3092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9490
_reflns_number_total             11469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09319j2.cif
_cod_data_source_block           frs087_150k_0m
_cod_database_code               7242203
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.443
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H51A,H51B} of C51, {H61A,H61B} of C61, {H53A,H53B} of C53,
   {H55A,H55B} of C55, {H57A,H57B} of C57
 At 1.5 times of:
  All C(H,H,H) groups, {H59A,H59B} of C59
2. Restrained distances
 C58-C57 = C55-C56 = C52-C51 = C53-C54 = C62-C61
 1.5 with sigma of 0.005
 O3-C61 = O5-C57 = O5-C55 = O6-C53 = O6-C51
 1.42 with sigma of 0.005
 C58-C57 = C55-C56 = C62-C61 = C60-C59
 1.5 with sigma of 0.005
 O2-C59 = O3-C61 = O6-C51 = O6-C53 = O5-C57 = O5-C55
 1.45 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C23) = Uanis(C25) = Uanis(C24) = Uanis(C22) = Uanis(C18) = Uanis(C20) =
Uanis(C21) = Uanis(C17)
Uanis(C57) = Uanis(C58) = Uanis(C56) = Uanis(C55)
Uanis(C62) = Uanis(C61) = Uanis(C59) = Uanis(C60)
Uanis(C51) = Uanis(C52) = Uanis(C54) = Uanis(C53)
4. Others
 Fixed Sof: C65(0.5) N7(0.5) C36(0.75) H36(0.75) C38(0.75) H38(0.75) C35(0.75)
 H35(0.75) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) C39(0.75) H39(0.75) C51(0.5)
 H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C17(0.5) H17(0.5)
 C21(0.5) H21(0.5) C57(0.5) H57A(0.5) H57B(0.5) C63(0.5) C18(0.5) H18(0.5)
 C20(0.5) H20(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) N8(0.5) C58(0.5)
 H58A(0.5) H58B(0.5) H58C(0.5) C53(0.5) H53A(0.5) H53B(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) H56C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C43(0.25) H43(0.25)
 C42(0.25) H42(0.25) C41(0.25) H41(0.25) C40(0.25) H40(0.25) C55(0.5) H55A(0.5)
 H55B(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C23(0.5) H23(0.5) C22(0.5)
 H22(0.5)
5.a Riding coordinates:
 C52(H52A,H52B,H52C), C62(H62A,H62B,H62C), C54(H54A,H54B,H54C), C60(H60A,H60B,
 H60C), C59(H59A,H59B)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C61(H61A,H61B), C57(H57A,H57B), C53(H53A,H53B), C55(H55A,H55B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C32(H32), C7(H7), C15(H15), C3(H3), C50(H50), C26(H26), C49(H49),
 C1(H1), C47(H47), C4(H4), C14(H14), C12(H12), C2(H2), C44(H44), C13(H13),
 C29(H29), C48(H48), C28(H28), C27(H27), C36(H36), C38(H38), C35(H35), C39(H39),
  C17(H17), C21(H21), C18(H18), C20(H20), C43(H43), C42(H42), C41(H41),
 C40(H40), C24(H24), C25(H25), C23(H23), C22(H22)
5.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C64(H64A,H64B,H64C), C58(H58A,H58B,H58C), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              29813
_olex2_date_sample_data_collection 2020-08-14
_olex2_date_sample_submission    2020-06-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
;
The crystal was mounted on a mylar loop in perfluoroether oil
;
_olex2_submission_original_sample_id FRS087_150K
_olex2_submission_special_instructions 'No special instructions were received'