Synthesis and reactivity of NHC-based rhodium macrocycles.
Andrew, Rhiann E.; Chaplin, Adrian B.; Inorganic chemistry 54 (2015) 312–322; doi:10.1021/ic5024828

data_4350710
_publ_section_title
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 Synthesis and reactivity of NHC-based rhodium macrocycles.
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_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              312
_journal_page_last               322
_journal_paper_doi               10.1021/ic5024828
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C26 H34 N5 O Rh, C2 H2'
_chemical_formula_sum            'C28 H36 N5 O Rh'
_chemical_formula_weight         561.53
_chemical_melting_point          ?
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-09
_audit_creation_method
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Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   19.2242(2)
_cell_length_b                   19.2242(2)
_cell_length_c                   37.5121(8)
_cell_measurement_reflns_used    35020
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0490
_cell_measurement_theta_min      2.9770
_cell_volume                     12006.0(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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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      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_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0025837000
_diffrn_orient_matrix_UB_12      -0.0192128000
_diffrn_orient_matrix_UB_13      0.0156723000
_diffrn_orient_matrix_UB_21      -0.0294238000
_diffrn_orient_matrix_UB_22      -0.0377054000
_diffrn_orient_matrix_UB_23      -0.0069419000
_diffrn_orient_matrix_UB_31      0.0307078000
_diffrn_orient_matrix_UB_32      -0.0049612000
_diffrn_orient_matrix_UB_33      -0.0079684000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            89168
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.373
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.978
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5256
_exptl_crystal_recrystallization_method
'Crystals grown from C6H6-pentane at 298 K'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.752
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5442
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0509P)^2^+25.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4905
_reflns_number_total             5442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5024828_si_002.cif
_cod_data_source_block           5-0040abc13
_cod_depositor_comments
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The following automatic conversions were performed:

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

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_cell_volume        12006.0(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4350710
_shelxl_version_number           2013-4
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C38-C37 \\sim C38-C37A \\sim C37-C36 \\sim C37A-C36A \\sim C36A-C35A \\sim
C36-C35 \\sim C35A-C34A ~
 C35-C34 \\sim C34-C33 \\sim C34A-C33A \\sim C33-C32 \\sim C33A-C32A \\sim
C32A-C31A \\sim C32-C31 ~
 C31-C30 \\sim C31A-C30A \\sim C30A-C29 \\sim C30-C29
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C30 \\sim C30A \\sim C31 \\sim C31A \\sim C32 \\sim C32A \\sim C33 \\sim C33A
\\sim C34 \\sim C34A \\sim C35 \\sim C35A \\sim C36A \\sim C36 \\sim C37 \\sim
C37A \\sim C38: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C31A)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C33A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H29C)=Sof(H29D)=Sof(H38C)=Sof(H38D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=
 Sof(H32C)=Sof(H32D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C34A)=Sof(H34C)=
 Sof(H34D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H38A)=Sof(H38B)=Sof(C37)=
 Sof(H37A)=Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C39(H39A,H39B), C29(H29A,H29B), C29(H29C,H29D), C30(H30A,
 H30B), C28(H28A,H28B), C38(H38A,H38B), C38(H38C,H38D), C37(H37A,H37B),
 C36(H36A,H36B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B), C34(H34A,H34B),
  C35(H35A,H35B), C36A(H36C,H36D), C35A(H35C,H35D), C31A(H31C,H31D), C32A(H32C,
 H32D), C37A(H37C,H37D), C34A(H34C,H34D), C33A(H33C,H33D), C30A(H30C,H30D)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C27(H27), C26(H26), C16(H16), C21(H21),
 C20(H20), C901(H901), C900(H900)
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_smtbx_masks_special_details
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The void contains a highly disordered pentane molecule on 
a special position.
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