Rotaxane synthesis exploiting the M( <scp>i</scp> )/M( <scp>iii</scp> ) redox couple
Emerson-King, Jack; Knighton, Richard C.; Gyton, Matthew R.; Chaplin, Adrian B.; Dalton Transactions 46 (2017) 11645–11655; doi:10.1039/C7DT02648J

data_1546829
_publ_section_title
;
 Rotaxane synthesis exploiting the M( <scp>i</scp> )/M( <scp>iii</scp> )
 redox couple
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              11645
_journal_page_last               11655
_journal_paper_doi               10.1039/C7DT02648J
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C72 H60 P4 Rh2, 2(C32 H12 B F24), C6 H14'
_chemical_formula_sum            'C142 H98 B2 F48 P4 Rh2'
_chemical_formula_weight         3067.52
_chemical_melting_point          ?
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                105.7768(16)
_cell_angle_beta                 101.1927(15)
_cell_angle_gamma                103.1955(17)
_cell_formula_units_Z            1
_cell_length_a                   13.2601(3)
_cell_length_b                   14.7604(3)
_cell_length_c                   18.6577(3)
_cell_measurement_reflns_used    31941
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.6150
_cell_measurement_theta_min      3.5080
_cell_volume                     3291.04(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00   1.00   1.00    6.50    --  -23.31 -37.00  30.00   99
  2  \w    -99.00   9.00   1.00    6.50    --  -23.31 -77.00 120.00  108
  3  \w      0.00  99.00   1.00    6.50    --   24.25  37.00-180.00   99
  4  \w      0.00  99.00   1.00    6.50    --   24.25  37.00  90.00   99
  5  \w     -8.00 100.00   1.00    6.50    --   24.25  77.00  60.00  108
  6  \w     -4.00  97.00   1.00    6.50    --   24.25  57.00 -30.00  101
  7  \w    -52.00  57.00   1.00    6.50    --   24.25 -77.00-150.00  109
  8  \w   -110.00 -55.00   1.00    6.50    --  -23.31 178.00 -90.00   55
  9  \w   -112.00 -87.00   1.00    6.50    --  -23.31-178.00   0.00   25
 10  \w    -48.00  52.00   1.00    6.50    --   24.25 -57.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0316579000
_diffrn_orient_matrix_UB_12      0.0326544000
_diffrn_orient_matrix_UB_13      -0.0009974000
_diffrn_orient_matrix_UB_21      0.0079194000
_diffrn_orient_matrix_UB_22      0.0124246000
_diffrn_orient_matrix_UB_23      0.0405943000
_diffrn_orient_matrix_UB_31      0.0468780000
_diffrn_orient_matrix_UB_32      0.0389278000
_diffrn_orient_matrix_UB_33      0.0061507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.102
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1542
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-hexane at 293 K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.347
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.071
_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     1005
_refine_ls_number_reflns         14464
_refine_ls_number_restraints     525
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0448P)^2^+4.3224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12826
_reflns_number_total             14464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02648j2.cif
_cod_data_source_block           0308abc17s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3291.04(11)
_cod_database_code               1546829
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F1A \\sim C207-F2A \\sim
C207-F3A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.01
 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim
C203-F3A
 with sigma of 0.01
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim
C208-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim
C205-F6A
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim
C232-F24A
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim
F24A-F22A
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim
C229-F24A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C92 \\sim C91 \\sim C90 \\sim F18 \\sim F16 \\sim F10 \\sim F11 \\sim F12 \\sim
F19 \\sim F21 \\sim F17 \\sim F20 \\sim F15 \\sim F1 \\sim F14 \\sim F13 \\sim
F2 \\sim F8 \\sim F6 \\sim F5 \\sim F4 \\sim F24 \\sim F23 \\sim F3 \\sim F7
\\sim F22 \\sim F9 \\sim F1A \\sim F2A \\sim F3A \\sim F5A \\sim F6A \\sim F4A
\\sim F7A \\sim F9A \\sim F8A \\sim F23A \\sim F24A \\sim F22A: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C92) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F12) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F17)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F14) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq,
Uanis(F24) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F1A) \\sim Ueq,
Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A)
\\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F9A) \\sim Ueq,
Uanis(F8A) \\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24A) \\sim Ueq, Uanis(F22A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(2)
 Sof(F6)=Sof(F5)=Sof(F4)=FVAR(2)
 Sof(F7A)=Sof(F9A)=Sof(F8A)=1-FVAR(3)
 Sof(F8)=Sof(F7)=Sof(F9)=FVAR(3)
 Sof(F23A)=Sof(F24A)=Sof(F22A)=1-FVAR(4)
 Sof(F24)=Sof(F23)=Sof(F22)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C90(H90A,H90B)
5.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C33(H33), C35(H35), C37(H37), C210(H210), C222(H222), C67(H67),
 C206(H206), C54(H54), C218(H218), C59(H59), C53(H53), C63(H63), C40(H40),
 C39(H39), C214(H214), C43(H43), C57(H57), C69(H69), C65(H65), C68(H68),
 C45(H45), C55(H55), C228(H228), C212(H212), C56(H56), C220(H220), C34(H34),
 C48(H48), C49(H49), C226(H226), C60(H60), C47(H47), C46(H46), C202(H202),
 C230(H230), C62(H62), C42(H42), C61(H61), C41(H41), C204(H204), C66(H66)
5.c Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C)
;
_shelx_res_checksum              35353
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.491
_oxdiff_exptl_absorpt_empirical_full_min 0.647