M24+ paddlewheel clusters as junction points in single-chain nanoparticles
Knöfel, Nicolai D.; Rothfuss, Hannah; Barner-Kowollik, Christopher; Roesky, Peter W.; Polymer Chemistry 10 (2019) 86–; doi:10.1039/C8PY01486H

data_1550218
_publ_section_title
;
 M24+ paddlewheel clusters as junction points in single-chain
 nanoparticles
;
_journal_issue                   1
_journal_name_full               'Polymer Chemistry'
_journal_page_first              86
_journal_paper_doi               10.1039/C8PY01486H
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C40 H36 D12 Mo2 O10 S2, 2(C2 D6 O S)'
_chemical_formula_sum            'C44 H36 D24 Mo2 O12 S4'
_chemical_formula_weight         1125.18
_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             2018-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-16 deposited with the CCDC.
2018-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                67.91(3)
_cell_angle_beta                 88.31(3)
_cell_angle_gamma                67.80(3)
_cell_formula_units_Z            1
_cell_length_a                   10.066(2)
_cell_length_b                   11.500(2)
_cell_length_c                   12.806(3)
_cell_measurement_reflns_used    12414
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      1.73
_cell_volume                     1260.8(6)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017) 
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      210.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9552
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.116
_diffrn_reflns_theta_min         1.731
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_voltage           0
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.7940
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       fragment
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.349
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0439P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4214
_reflns_number_total             4916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01486h2.cif
_cod_data_source_block           nkca01abs
_cod_depositor_comments
'Adding full bibliography for 1550218--1550219.cif.'
_cod_original_cell_volume        1260.7(6)
_cod_database_code               1550218
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.713
_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
2. Others
 Fixed Sof: S1A(0.55) C19A(0.55) D19A(0.55) D19B(0.55) D19C(0.55) C20A(0.55)
 D20A(0.55) D20B(0.55) D20C(0.55) S2A(0.65) O6A(0.65) C21A(0.65) D21A(0.65)
 D21B(0.65) D21C(0.65) C22A(0.65) D22A(0.65) D22B(0.65) D22C(0.65) S1B(0.45)
 S2B(0.35) O6B(0.35) C19B(0.45) D19D(0.45) D19E(0.45) D19F(0.45) C20B(0.45)
 D20D(0.45) D20E(0.45) D20F(0.45) C21B(0.35) D21D(0.35) D21E(0.35) D21F(0.35)
 C22B(0.35) D22D(0.35) D22E(0.35) D22F(0.35)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C12(H12), C13(H13), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C19A(D19A,D19B,D19C), C20A(D20A,D20B,
 D20C), C21A(D21A,D21B,D21C), C22A(D22A,D22B,D22C), C19B(D19D,D19E,D19F),
 C20B(D20D,D20E,D20F), C21B(D21D,D21E,D21F), C22B(D22D,D22E,D22F)
;
_shelx_res_checksum              84534
_olex2_submission_special_instructions 'No special instructions were received'