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_7039228
_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         'C64 H80 I2 N4 O4 Rh2'
_chemical_formula_sum            'C64 H80 I2 N4 O4 Rh2'
_chemical_formula_weight         1428.94
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-27
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
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_audit_update_record
;
2016-01-21 deposited with the CCDC.
2016-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4834(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.07898(15)
_cell_length_b                   27.7640(3)
_cell_length_c                   17.30754(19)
_cell_measurement_reflns_used    29712
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.2730
_cell_measurement_theta_min      2.5750
_cell_volume                     6198.91(12)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_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      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   35.00  113.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  178.0000 -120.0000 78

  2 omega   35.00  113.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653  178.0000  -30.0000 78

  3 omega  -10.00  102.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   77.0000    0.0000 112

  4 omega -114.00  -57.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590 -178.0000 -120.0000 57

  5 omega  -51.00   52.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2590   38.0000  150.0000 103

  6 omega   -3.00   33.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   38.0000  -90.0000 36

  7 omega  -10.00  102.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1653   77.0000  150.0000 112
;
_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      -0.0236160000
_diffrn_orient_matrix_UB_12      0.0102406000
_diffrn_orient_matrix_UB_13      -0.0361086000
_diffrn_orient_matrix_UB_21      -0.0103845000
_diffrn_orient_matrix_UB_22      -0.0234063000
_diffrn_orient_matrix_UB_23      -0.0157770000
_diffrn_orient_matrix_UB_31      -0.0485435000
_diffrn_orient_matrix_UB_32      0.0000219000
_diffrn_orient_matrix_UB_33      0.0131944000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75467
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.372
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.935
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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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    1.531
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.053
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         12663
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.3162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10426
_reflns_number_total             12663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01001f2.cif
_cod_data_source_block           0123abc14
_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        6198.92(12)
_cod_database_code               7039228
_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
 O61-C62A \\sim O61-C62 \\sim O69-C70 \\sim O69-C70A
 with sigma of 0.01
 C71-C70 \\sim C71A-C70A \\sim C72-C71 \\sim C72A-C71A \\sim C63-C62 \\sim
C63A-C62A \\sim C64-C63 ~
 C64A-C63A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O61 \\sim C62A \\sim C63A \\sim C64A \\sim C62 \\sim C64 \\sim C63 \\sim O69
\\sim C70A \\sim C71A \\sim C72A \\sim C70 \\sim C71 \\sim C72: within 1.7A
with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(O61) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C63A) \\sim Ueq, Uanis(C64A)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(O69) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C71A) \\sim Ueq, Uanis(C72A)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq:
with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(C62A) = Uanis(C62)
Uanis(C63) = Uanis(C63A)
Uanis(C70) = Uanis(C70A)
Uanis(C71) = Uanis(C71A)
Uanis(C64) = Uanis(C64A)
Uanis(C72) = Uanis(C72A)
4. Others
 Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C72A)=
 Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(1)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=
 Sof(H72B)=Sof(H72C)=FVAR(1)
 Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C64A)=
 Sof(H64D)=Sof(H64E)=Sof(H64F)=1-FVAR(2)
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=
 Sof(H64B)=Sof(H64C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14), C17(H17), C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B),
 C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B), C39(H39A,H39B), C46(H46A,H46B),
  C53(H53A,H53B), C60(H60A,H60B), C62(H62A,H62B), C62A(H62C,H62D), C63(H63A,
 H63B), C63A(H63C,H63D), C66(H66A,H66B), C67(H67A,H67B), C70(H70A,H70B),
 C70A(H70C,H70D), C71(H71A,H71B), C71A(H71C,H71D), C74(H74A,H74B), C75(H75A,
 H75B)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C29(H29), C30(H30), C34(H34), C38(H38), C40(H40),
 C41(H41), C45(H45), C48(H48), C52(H52), C54(H54), C55(H55), C59(H59)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C64(H64A,H64B,H64C), C64A(H64D,H64E,
 H64F), C68(H68A,H68B,H68C), C72(H72A,H72B,H72C), C72A(H72D,H72E,H72F),
 C76(H76A,H76B,H76C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'