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_7039233
_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         'C52 H56 Cl N4 O8 Rh2, C32 H12 B F24'
_chemical_formula_sum            'C84 H68 B Cl F24 N4 O8 Rh2'
_chemical_formula_weight         1969.50
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 109.352(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6345(4)
_cell_length_b                   22.6778(5)
_cell_length_c                   20.0799(4)
_cell_measurement_reflns_used    9609
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.0490
_cell_measurement_theta_min      3.8850
_cell_volume                     8435.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXT (Sheldrick, 2015)'
_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  -50.00   33.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109   38.0000  -90.0000 83

  2 omega  -50.00   33.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109   38.0000  120.0000 83

  3 omega -115.00  -14.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109  -57.0000 -180.0000 101

  4 omega   18.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7109 -125.0000   60.0000 80

  5 omega   38.00  116.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  -90.0000 78

  6 omega   61.00  178.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000   30.0000 117

  7 omega  100.00  178.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  111.0000 -150.0000 78

  8 omega   42.00  143.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -61.0000  120.0000 101

  9 omega   38.00   91.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000 -120.0000 53

 10 omega   38.00  116.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  120.0000 78

 11 omega   38.00   91.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000 -180.0000 53

 12 omega   41.00   98.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000  -60.0000 57

 13 omega -115.00  -40.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109  -57.0000  -30.0000 75
;
_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      0.0150700000
_diffrn_orient_matrix_UB_12      0.0611709000
_diffrn_orient_matrix_UB_13      0.0353469000
_diffrn_orient_matrix_UB_21      0.0285786000
_diffrn_orient_matrix_UB_22      -0.0295281000
_diffrn_orient_matrix_UB_23      0.0730477000
_diffrn_orient_matrix_UB_31      0.0766510000
_diffrn_orient_matrix_UB_32      -0.0008036000
_diffrn_orient_matrix_UB_33      -0.0049429000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46355
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         17.151
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.330
_refine_ls_extinction_coef       0.0001(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   2.559
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1224
_refine_ls_number_reflns         14873
_refine_ls_number_restraints     1923
_refine_ls_restrained_S_all      2.454
_refine_ls_R_factor_all          0.2973
_refine_ls_R_factor_gt           0.2744
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6103
_refine_ls_wR_factor_ref         0.6304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11268
_reflns_number_total             14873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01001f2.cif
_cod_data_source_block           0150abc15
_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_database_code               7039233
_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
 O9-C8 \\sim O11-C10 \\sim O5-C4 \\sim O7-C6 \\sim C6A-O7A
 with sigma of 0.005
 Rh1-C4 \\sim Rh1-C6 \\sim Rh2-C8 \\sim Rh2-C10 \\sim Rh1-C6A
 with sigma of 0.005
 Rh1-C12 \\sim Rh2-C18
 with sigma of 0.005
 Rh1-Cl3 \\sim Rh2-Cl3
 with sigma of 0.005
 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
 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
 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
 N19-C18 \\sim N22-C18 \\sim N13-C12 \\sim N16-C12
 with sigma of 0.001
3. Restrained planarity
 Rh1, Cl3, O5, O7, C4, C6, C12
 with sigma of 0.007
 Rh2, Cl3, O9, O11, C8, C10, C18
 with sigma of 0.007
 Rh1, Rh2, Cl3, O7, O7A, O11, C6, C6A, C10
 with sigma of 0.007
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Others
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Fixed Sof: O7(0.5) O7A(0.5) C6(0.5) C6A(0.5) F4(0.5) F4A(0.5) F5(0.5)
 F5A(0.5) F6(0.5) F6A(0.5) F13(0.5) F13A(0.5) F14(0.5) F14A(0.5) F15(0.5)
 F15A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C37(H37A,H37B), C44(H44A,H44B), C51(H51A,H51B), C53(H53A,
 H53B), C54(H54A,H54B), C57(H57A,H57B), C58(H58A,H58B), C61(H61A,H61B),
 C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C20(H20), C21(H21), C25(H25), C29(H29), C31(H31),
 C32(H32), C36(H36), C39(H39), C43(H43), C45(H45), C46(H46), C50(H50),
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C55(H55A,H55B,H55C), C59(H59A,H59B,
 H59C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'