Coordination chemistry of a calix[4]arene-based NHC ligand: dinuclear complexes and comparison to I(i)Pr2Me2.
Patchett, Ruth; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8945–8955; doi:10.1039/c6dt01001f

data_7039234
_publ_section_title
;
 Coordination chemistry of a calix[4]arene-based NHC ligand: dinuclear
 complexes and comparison to I(i)Pr2Me2.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8945
_journal_page_last               8955
_journal_paper_doi               10.1039/c6dt01001f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C26 H40 Cl N4 O4 Rh2, C32 H12 B F24'
_chemical_formula_sum            'C58 H52 B Cl F24 N4 O4 Rh2'
_chemical_formula_weight         1577.11
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.9872(15)
_cell_angle_beta                 94.9257(17)
_cell_angle_gamma                91.7507(18)
_cell_formula_units_Z            2
_cell_length_a                   12.2319(3)
_cell_length_b                   13.2693(3)
_cell_length_c                   21.7143(4)
_cell_measurement_reflns_used    28513
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.3530
_cell_measurement_theta_min      3.3440
_cell_volume                     3443.07(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   32.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653 -178.0000  150.0000 80

  2 omega   35.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  178.0000 -180.0000 78

  3 omega   35.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  178.0000  -90.0000 78

  4 omega  -10.00  102.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   77.0000 -120.0000 112

  5 omega -103.00    9.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -77.0000  -30.0000 112

  6 omega  -54.00   50.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590   57.0000  -60.0000 104

  7 omega -113.00  -53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  178.0000 -180.0000 60

  8 omega  -58.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590   77.0000 -180.0000 112

  9 omega  -25.00    0.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  -99.0000  150.0000 25

 10 omega   -6.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   57.0000   90.0000 103

 11 omega  -93.00  -30.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  144.0000  -74.0000 63

 12 omega  -51.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590   38.0000   30.0000 103

 13 omega  -98.00    5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590  -57.0000   90.0000 103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0301714000
_diffrn_orient_matrix_UB_12      -0.0448355000
_diffrn_orient_matrix_UB_13      -0.0073933000
_diffrn_orient_matrix_UB_21      -0.0091317000
_diffrn_orient_matrix_UB_22      0.0014243000
_diffrn_orient_matrix_UB_23      -0.0325186000
_diffrn_orient_matrix_UB_31      0.0490066000
_diffrn_orient_matrix_UB_32      0.0309781000
_diffrn_orient_matrix_UB_33      0.0022056000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            133482
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.372
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
)
TITL 0105abc14
CELL   12.2319   13.2693   21.7143    100.99     94.93     91.75
SPGR P-1
C101 0.573 0.374 0.543 !       2.68 eA-3
C102 0.500 0.500 0.500 !       2.02 eA-3
C103 0.423 0.581 0.485 !       1.35 eA-3
Q104 0.952 0.863 0.749 !       1.26 eA-3
Q105 0.359 0.905 0.103 !       1.13 eA-3
Q106 0.175 1.004 0.865 !       1.02 eA-3
Q107 0.064 0.767 0.757 !       0.87 eA-3
Q108 0.933 0.440 0.708 !       0.86 eA-3
Q109 0.198 0.325 0.889 !       0.84 eA-3
Q110 0.215 0.587 0.965 !       0.84 eA-3
Q111 0.254 0.042 0.759 !       0.81 eA-3
Q112 0.858 0.519 0.364 !       0.81 eA-3
Q113 0.690 0.050 0.283 !       0.80 eA-3
Q114 0.113 0.604 0.353 !       0.79 eA-3
Q115 0.116 0.658 0.068 !       0.76 eA-3
Q116 0.892 0.271 0.192 !       0.75 eA-3
Q117 0.918 0.750 0.188 !       0.74 eA-3
Q118 0.471 0.951 0.811 !       0.72 eA-3
Q119 0.322 0.900 0.968 !       0.70 eA-3
Q120 0.392 0.252 0.360 !       0.67 eA-3
Q121 0.472 0.717 0.936 !       0.66 eA-3
Q122 0.986 0.908 0.771 !       0.66 eA-3
Q123 0.763 0.967 0.077 !       0.66 eA-3
Q124 0.380 0.287 0.970 !       0.65 eA-3
Q125 0.425 0.063 0.191 !       0.60 eA-3
Q126 0.475 0.687 0.011 !       0.60 eA-3
Q127 0.639 0.999 0.841 !       0.59 eA-3
Q128 0.485 0.746 0.743 !       0.59 eA-3
Q129 0.063 0.453 0.332 !       0.59 eA-3
Q130 0.242 0.916 0.907 !       0.58 eA-3
Q131 0.888 0.403 0.981 !       0.57 eA-3
Q132 0.558 0.294 0.338 !       0.57 eA-3
Q133 0.859 0.672 0.408 !       0.55 eA-3
Q134 0.708 1.000 0.310 !       0.55 eA-3
Q135 0.625 0.614 0.680 !       0.54 eA-3
Q136 0.044 0.230 0.037 !       0.54 eA-3
Q137 0.501 0.689 0.626 !       0.54 eA-3
Q138 0.455 0.341 0.961 !       0.54 eA-3
Q139 0.889 0.510 0.609 !       0.53 eA-3
Q140 0.783 0.652 0.236 !       0.53 eA-3
Q141 0.153 0.406 0.892 !       0.52 eA-3
Q142 0.281 0.407 0.586 !       0.51 eA-3
Q143 0.609 0.755 0.963 !       0.51 eA-3
Q144 0.615 0.974 0.598 !       0.51 eA-3
Q145 0.706 0.981 0.843 !       0.50 eA-3
)
;
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         14061
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+2.6446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11271
_reflns_number_total             14061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01001f2.cif
_cod_data_source_block           0105abc14
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039227--7039236.cif.
;
_cod_original_cell_volume        3443.08(12)
_cod_database_code               7039234
_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
 N16-C21 \\sim N16-C121 \\sim N29-C34 \\sim N29-C134 \\sim N16-C22 \\sim N29-C35
 with sigma of 0.005
 N29-C35 \\sim N29-C134 \\sim N29-C34
 with sigma of 0.005
 C35-C134 \\sim C35-C34 \\sim C22-C21 \\sim C22-C121
 with sigma of 0.005
 C134-C33 \\sim C34-C33 \\sim C35-C33 \\sim C21-C20 \\sim C121-C20 \\sim C22-C20
 with sigma of 0.005
 N29-C33 \\sim N16-C20
 with sigma of 0.005
 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
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim
C216-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim
C213-F12A
 with sigma of 0.01
 C223-F13 \\sim C223-F14 \\sim C223-F15 \\sim C223-F13A \\sim C223-F14A \\sim
C223-F15A
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F13A-F14A \\sim F14A-F15A \\sim
F15A-F13A
 with sigma of 0.01
 C219-F13 \\sim C219-F14 \\sim C219-F15 \\sim C219-F13A \\sim C219-F14A \\sim
C219-F15A
 with sigma of 0.01
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim
C231-F21A
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim
F21A-F19A
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim
C227-F21A
 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
C134 \\sim C34 \\sim C33 \\sim C20 \\sim C21 \\sim C121 \\sim C22 \\sim C35
\\sim F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F5
\\sim F6 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F10A \\sim F11 \\sim F11A
\\sim F12 \\sim F12A \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim
F15A \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F19A \\sim F20 \\sim F20A
\\sim F21 \\sim F21A \\sim F22 \\sim F22A \\sim F23 \\sim F23A \\sim F24 \\sim
F24A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C134) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq,
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq,
Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq,
Uanis(F14) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F15A)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq,
Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A)
\\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22) \\sim Ueq,
Uanis(F22A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24)
\\sim Ueq, Uanis(F24A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.02
Uanis(C134) = Uanis(C34)
Uanis(C121) = Uanis(C21)
Uanis(F15) = Uanis(F15A)
4. Others
 Sof(H33A)=Sof(C134)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(1)
 Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(H20A)=Sof(C121)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(2)
 Sof(H20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(3)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(3)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(4)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(4)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(5)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(5)
 Fixed Sof: F10(0.5) F10A(0.5) F11(0.5) F11A(0.5) F12(0.5) F12A(0.5) F22(0.5)
 F22A(0.5) F23(0.5) F23A(0.5) F24(0.5) F24A(0.5)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C20(H20A), C30(H30), C33(H33), C33(H33A)
5.b Aromatic/amide H refined with riding coordinates:
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C121(H12A,H12B,H12C), C134(H13A,H13B,H13C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'