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_7242204
_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
'C42 H32 N6 O6 P2 Rh, 4.25(N O3), 1.25(H3 O), 2.75(H2 O)'
_chemical_formula_sum            'C42 H41.25 N10.25 O22.75 P2 Rh'
_chemical_formula_weight         1218.45
_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             2020-10-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-23 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                91.845(2)
_cell_angle_beta                 110.580(2)
_cell_angle_gamma                110.494(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5277(7)
_cell_length_b                   14.3560(8)
_cell_length_c                   15.7458(9)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.067
_cell_measurement_theta_min      4.042
_cell_volume                     2444.1(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.952
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23158
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.272
_diffrn_reflns_theta_min         3.339
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.300
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0629 before and 0.0336 after correction.
The Ratio of minimum to maximum transmission is 0.7994.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.814
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8879
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0729P)^2^+9.2056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8743
_reflns_number_total             8879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09319j2.cif
_cod_data_source_block           frs_150k_0m
_cod_database_code               7242204
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.512
_shelx_estimated_absorpt_t_min   0.465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 N11-O24 \\sim N11-O25 \\sim N11-O20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O20A) = Uiso(O25) = Uiso(O24)
4. Others
 Fixed Sof: O20(0.35) H9(0.35) H10(0.35) O21(0.4) H11(0.4) H12(0.4) O22(0.5)
 H13(0.5) H14(0.5) O23(0.25) H15(0.25) H16(0.25) O27(0.25) H17(0.25) H18(0.25)
 O28(0.25) H19(0.25) H20(0.25) H21(0.25) N11(0.25) O24(0.25) O25(0.25)
 O20A(0.25) O26(0.5) H22(0.5) H23(0.5) O29(0.5) H24(0.5) H25(0.5)
5.a Riding coordinates:
 O19(H4,H5,H6), O20(H9), O20(H10), O21(H11), O21(H12), O22(H13), O22(H14),
 O23(H15), O23(H16), O27(H17), O27(H18), O28(H19,H20,H21), O26(H22), O26(H23),
 O29(H24), O29(H25)
5.b Aromatic/amide H refined with riding coordinates:
 C9(HD), C22(HE), C4(HF), C24(HG), C15(HH), C25(HI), C14(HJ), C3(HK), C43(HL),
 C7(HM), C30(HN), C23(HO), C18(HP), C1(HQ), C2(HR), C12(HS), C20(HT), C17(HU),
 C21(HV), C33(HW), C13(HX), C36(HY), C39(HZ), C38(H1), C35(H2), C34(H3),
 C42(H7), C41(H8)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H), O4(HA), O3(HB), O5(HC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22299
_olex2_date_sample_data_collection 2020-10-17
_olex2_date_sample_submission    2020-09-11
_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 FRS86
_olex2_submission_special_instructions 'No special instructions were received'