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_7039236
_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         'C24 H40 N4 O2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C56 H52 B F24 N4 O2 Rh'
_chemical_formula_weight         1382.73
_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                79.1970(13)
_cell_angle_beta                 87.6582(15)
_cell_angle_gamma                76.3505(14)
_cell_formula_units_Z            4
_cell_length_a                   17.0878(3)
_cell_length_b                   18.9928(3)
_cell_length_c                   19.5695(4)
_cell_measurement_reflns_used    32281
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3030
_cell_measurement_theta_min      3.5580
_cell_volume                     6062.40(19)
_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  -59.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1793  -38.0000  -60.0000 103

  2 omega  -72.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1793    0.0000 -180.0000 179

  3 omega   35.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1793  178.0000  -90.0000 72

  4 omega  -25.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1793  -99.0000   90.0000 84

  5 omega  -25.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2730  -99.0000  -90.0000 49

  6 omega  -77.00  -21.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2730  128.0000 -172.0000 56

  7 omega   -9.00   27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1793   38.0000  -90.0000 36

  8 omega   -9.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1793   38.0000   30.0000 102

  9 omega  -25.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2730  -99.0000   30.0000 49

 10 omega  -25.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2730  -99.0000   90.0000 49

 11 omega  -92.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2730  -57.0000 -150.0000 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      -0.0211383000
_diffrn_orient_matrix_UB_12      0.0078038000
_diffrn_orient_matrix_UB_13      -0.0320036000
_diffrn_orient_matrix_UB_21      -0.0370427000
_diffrn_orient_matrix_UB_22      0.0035846000
_diffrn_orient_matrix_UB_23      0.0182469000
_diffrn_orient_matrix_UB_31      -0.0023789000
_diffrn_orient_matrix_UB_32      0.0381370000
_diffrn_orient_matrix_UB_33      -0.0020921000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            124137
_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         3.306
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89795
_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    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1806
_refine_ls_number_reflns         24757
_refine_ls_number_restraints     1056
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0521P)^2^+5.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19586
_reflns_number_total             24757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01001f2.cif
_cod_data_source_block           0080abc14
_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        6062.41(18)
_cod_database_code               7039236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C207-F201 \\sim C207-F202 \\sim C207-F203 \\sim C207-F301 \\sim C207-F302
\\sim C207-F303
 with sigma of 0.01
 F201-F202 \\sim F202-F203 \\sim F203-F201 \\sim F301-F302 \\sim F302-F303
\\sim F303-F301
 with sigma of 0.01
 C203-F201 \\sim C203-F202 \\sim C203-F203 \\sim C203-F301 \\sim C203-F302
\\sim C203-F303
 with sigma of 0.01
 C216-F210 \\sim C216-F211 \\sim C216-F212 \\sim C216-F310 \\sim C216-F311
\\sim C216-F312
 with sigma of 0.01
 F210-F211 \\sim F211-F212 \\sim F212-F210 \\sim F310-F311 \\sim F311-F312
\\sim F312-F310
 with sigma of 0.01
 C213-F210 \\sim C213-F211 \\sim C213-F212 \\sim C213-F310 \\sim C213-F311
\\sim C213-F312
 with sigma of 0.01
 C231-F219 \\sim C231-F220 \\sim C231-F221 \\sim C231-F319 \\sim C231-F320
\\sim C231-F321
 with sigma of 0.01
 F219-F220 \\sim F220-F221 \\sim F221-F219 \\sim F319-F320 \\sim F320-F321
\\sim F321-F319
 with sigma of 0.01
 C227-F219 \\sim C227-F220 \\sim C227-F221 \\sim C227-F319 \\sim C227-F320
\\sim C227-F321
 with sigma of 0.01
 C407-F401 \\sim C407-F402 \\sim C407-F403 \\sim C407-F501 \\sim C407-F502
\\sim C407-F503
 with sigma of 0.01
 F401-F402 \\sim F402-F403 \\sim F403-F401 \\sim F501-F502 \\sim F502-F503
\\sim F503-F501
 with sigma of 0.01
 C403-F401 \\sim C403-F402 \\sim C403-F403 \\sim C403-F501 \\sim C403-F502
\\sim C403-F503
 with sigma of 0.01
 C415-F407 \\sim C415-F408 \\sim C415-F409 \\sim C415-F507 \\sim C415-F508
\\sim C415-F509
 with sigma of 0.01
 F407-F408 \\sim F408-F409 \\sim F409-F407 \\sim F507-F508 \\sim F508-F509
\\sim F509-F507
 with sigma of 0.01
 C411-F407 \\sim C411-F408 \\sim C411-F409 \\sim C411-F507 \\sim C411-F508
\\sim C411-F509
 with sigma of 0.01
 C423-F413 \\sim C423-F414 \\sim C423-F415 \\sim C423-F513 \\sim C423-F514
\\sim C423-F515
 with sigma of 0.01
 F413-F414 \\sim F414-F415 \\sim F415-F413 \\sim F513-F514 \\sim F514-F515
\\sim F515-F513
 with sigma of 0.01
 C419-F413 \\sim C419-F414 \\sim C419-F415 \\sim C419-F513 \\sim C419-F514
\\sim C419-F515
 with sigma of 0.01
 C432-F422 \\sim C432-F423 \\sim C432-F424 \\sim C432-F522 \\sim C432-F523
\\sim C432-F524
 with sigma of 0.01
 F422-F423 \\sim F423-F424 \\sim F424-F422 \\sim F522-F523 \\sim F523-F524
\\sim F524-F522
 with sigma of 0.01
 C429-F422 \\sim C429-F423 \\sim C429-F424 \\sim C429-F522 \\sim C429-F523
\\sim C429-F524
 with sigma of 0.01
 C232-F222 \\sim C232-F223 \\sim C232-F224 \\sim C232-F322 \\sim C232-F323
\\sim C232-F324
 with sigma of 0.01
 F222-F223 \\sim F223-F224 \\sim F224-F222 \\sim F322-F323 \\sim F323-F324
\\sim F324-F322
 with sigma of 0.01
 C229-F222 \\sim C229-F223 \\sim C229-F224 \\sim C229-F322 \\sim C229-F323
\\sim C229-F324
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F201 \\sim F202 \\sim F203 \\sim F204 \\sim F205 \\sim F206 \\sim F207 \\sim
F208 \\sim F209 \\sim F210 \\sim F211 \\sim F212 \\sim F213 \\sim F214 \\sim
F215 \\sim F216 \\sim F217 \\sim F218 \\sim F219 \\sim F220 \\sim F221 \\sim
F222 \\sim F223 \\sim F224 \\sim F301 \\sim F302 \\sim F303 \\sim F310 \\sim
F311 \\sim F312 \\sim F319 \\sim F320 \\sim F321 \\sim F322 \\sim F323 \\sim
F324 \\sim F401 \\sim F402 \\sim F403 \\sim F404 \\sim F405 \\sim F406 \\sim
F407 \\sim F408 \\sim F409 \\sim F410 \\sim F411 \\sim F412 \\sim F413 \\sim
F414 \\sim F415 \\sim F416 \\sim F417 \\sim F418 \\sim F419 \\sim F420 \\sim
F421 \\sim F422 \\sim F423 \\sim F424 \\sim F501 \\sim F502 \\sim F503 \\sim
F507 \\sim F508 \\sim F509 \\sim F513 \\sim F514 \\sim F515 \\sim F522 \\sim
F523 \\sim F524: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F201) \\sim Ueq, Uanis(F202) \\sim Ueq, Uanis(F203) \\sim Ueq,
Uanis(F204) \\sim Ueq, Uanis(F205) \\sim Ueq, Uanis(F206) \\sim Ueq,
Uanis(F207) \\sim Ueq, Uanis(F208) \\sim Ueq, Uanis(F209) \\sim Ueq,
Uanis(F210) \\sim Ueq, Uanis(F211) \\sim Ueq, Uanis(F212) \\sim Ueq,
Uanis(F213) \\sim Ueq, Uanis(F214) \\sim Ueq, Uanis(F215) \\sim Ueq,
Uanis(F216) \\sim Ueq, Uanis(F217) \\sim Ueq, Uanis(F218) \\sim Ueq,
Uanis(F219) \\sim Ueq, Uanis(F220) \\sim Ueq, Uanis(F221) \\sim Ueq,
Uanis(F222) \\sim Ueq, Uanis(F223) \\sim Ueq, Uanis(F224) \\sim Ueq,
Uanis(F301) \\sim Ueq, Uanis(F302) \\sim Ueq, Uanis(F303) \\sim Ueq,
Uanis(F310) \\sim Ueq, Uanis(F311) \\sim Ueq, Uanis(F312) \\sim Ueq,
Uanis(F319) \\sim Ueq, Uanis(F320) \\sim Ueq, Uanis(F321) \\sim Ueq,
Uanis(F322) \\sim Ueq, Uanis(F323) \\sim Ueq, Uanis(F324) \\sim Ueq,
Uanis(F401) \\sim Ueq, Uanis(F402) \\sim Ueq, Uanis(F403) \\sim Ueq,
Uanis(F404) \\sim Ueq, Uanis(F405) \\sim Ueq, Uanis(F406) \\sim Ueq,
Uanis(F407) \\sim Ueq, Uanis(F408) \\sim Ueq, Uanis(F409) \\sim Ueq,
Uanis(F410) \\sim Ueq, Uanis(F411) \\sim Ueq, Uanis(F412) \\sim Ueq,
Uanis(F413) \\sim Ueq, Uanis(F414) \\sim Ueq, Uanis(F415) \\sim Ueq,
Uanis(F416) \\sim Ueq, Uanis(F417) \\sim Ueq, Uanis(F418) \\sim Ueq,
Uanis(F419) \\sim Ueq, Uanis(F420) \\sim Ueq, Uanis(F421) \\sim Ueq,
Uanis(F422) \\sim Ueq, Uanis(F423) \\sim Ueq, Uanis(F424) \\sim Ueq,
Uanis(F501) \\sim Ueq, Uanis(F502) \\sim Ueq, Uanis(F503) \\sim Ueq,
Uanis(F507) \\sim Ueq, Uanis(F508) \\sim Ueq, Uanis(F509) \\sim Ueq,
Uanis(F513) \\sim Ueq, Uanis(F514) \\sim Ueq, Uanis(F515) \\sim Ueq,
Uanis(F522) \\sim Ueq, Uanis(F523) \\sim Ueq, Uanis(F524) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.02
Uanis(F323) = Uanis(F222)
Uanis(F324) = Uanis(F223)
Uanis(F224) = Uanis(F322)
Uanis(F301) = Uanis(F201)
4. Others
 Sof(F310)=Sof(F311)=Sof(F312)=1-FVAR(1)
 Sof(F210)=Sof(F211)=Sof(F212)=FVAR(1)
 Sof(F301)=Sof(F302)=Sof(F303)=1-FVAR(2)
 Sof(F201)=Sof(F202)=Sof(F203)=FVAR(2)
 Sof(F319)=Sof(F320)=Sof(F321)=1-FVAR(3)
 Sof(F219)=Sof(F220)=Sof(F221)=FVAR(3)
 Sof(F513)=Sof(F514)=Sof(F515)=1-FVAR(4)
 Sof(F413)=Sof(F414)=Sof(F415)=FVAR(4)
 Sof(F522)=Sof(F523)=Sof(F524)=1-FVAR(5)
 Sof(F422)=Sof(F423)=Sof(F424)=FVAR(5)
 Fixed Sof: F222(0.5) F223(0.5) F224(0.5) F322(0.5) F323(0.5) F324(0.5)
 F401(0.5) F402(0.5) F403(0.5) F407(0.5) F408(0.5) F409(0.5) F501(0.5)
 F502(0.5) F503(0.5) F507(0.5) F508(0.5) F509(0.5)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C24(H24), C27(H27), C110(H110), C113(H113), C123(H123),
 C126(H126)
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),
 C402(H402), C404(H404), C406(H406), C410(H410), C412(H412), C414(H414),
 C418(H418), C420(H420), C422(H422), C426(H426), C428(H428), C430(H430)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C114(H11G,
 H11H,H11I), C115(H11J,H11K,H11L), C116(H11M,H11N,H11O), C117(H11P,H11Q,H11R),
 C124(H12D,H12E,H12F), C125(H12G,H12H,H12I), C127(H12J,H12K,H12L), C128(H12M,
 H12N,H12O), C129(H12P,H12Q,H12R), C130(H13D,H13E,H13F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'