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_4350705
_publ_section_title
;
 Synthesis and reactivity of NHC-based rhodium macrocycles.
;
_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 H35 N5 O Rh, C32 H12 B F24'
_chemical_formula_sum            'C58 H47 B F24 N5 O Rh'
_chemical_formula_weight         1399.72
_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'
_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                116.409(3)
_cell_angle_beta                 94.878(3)
_cell_angle_gamma                92.986(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3661(3)
_cell_length_b                   18.7809(6)
_cell_length_c                   19.3860(6)
_cell_measurement_reflns_used    8966
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1779
_cell_measurement_theta_min      3.1541
_cell_volume                     3027.65(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -16.00   83.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1593   57.0000 -180.0000 99

  2 omega  -83.00   15.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0968  -57.0000 -120.0000 98

  3 omega  -34.00   56.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0968   57.0000   30.0000 90

  4 omega   -1.00   28.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.0968  -99.0000    0.0000 29
;
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0192216000
_diffrn_orient_matrix_UB_12      -0.0417152000
_diffrn_orient_matrix_UB_13      -0.0155325000
_diffrn_orient_matrix_UB_21      -0.0718548000
_diffrn_orient_matrix_UB_22      0.0071583000
_diffrn_orient_matrix_UB_23      0.0079013000
_diffrn_orient_matrix_UB_31      -0.0174220000
_diffrn_orient_matrix_UB_32      -0.0022246000
_diffrn_orient_matrix_UB_33      -0.0372819000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23522
_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         26.372
_diffrn_reflns_theta_min         3.160
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'Crystals grown from Diethylether-Hexane at 298 K'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         12359
_refine_ls_number_restraints     852
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0411P)^2^+2.7726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9957
_reflns_number_total             12359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5024828_si_002.cif
_cod_data_source_block           1a-0010abc13
_cod_depositor_comments
;
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 
;
_cod_original_cell_volume        3027.66(18)
_cod_database_code               4350705
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C215-F7 \\sim C215-F8 \\sim C215-F9 \\sim C215-F107 \\sim C215-F108 \\sim
C215-F109
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F107-F108 \\sim F108-F109 \\sim F109-F107
 with sigma of 0.01
 C211-F7 \\sim C211-F8 \\sim C211-F9 \\sim C211-F107 \\sim C211-F108 \\sim
C211-F109
 with sigma of 0.01
 C213-C216 \\sim C213-C316
 with sigma of 0.01
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C307-F101 \\sim C307-F102 \\sim
C307-F103
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F101-F102 \\sim F102-F103 \\sim F103-F101
 with sigma of 0.01
 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F101 \\sim C203-F102 \\sim
C203-F103
 with sigma of 0.01
 C203-C207 \\sim C203-C307
 with sigma of 0.01
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C308-F104 \\sim C308-F105 \\sim
C308-F106
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F104-F105 \\sim F105-F106 \\sim F106-F104
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F104 \\sim C205-F105 \\sim
C205-F106
 with sigma of 0.01
 C205-C208 \\sim C205-C308
 with sigma of 0.01
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C316-F110 \\sim C316-F111 \\sim
C316-F112
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F110-F111 \\sim F111-F112 \\sim
F112-F110
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F110 \\sim C213-F111 \\sim
C213-F112
 with sigma of 0.01
 C213-C216 \\sim C213-C316
 with sigma of 0.01
 C223-F13 \\sim C223-F14 \\sim C223-F15 \\sim C223-F113 \\sim C223-F114 \\sim
C223-F115
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F113-F114 \\sim F114-F115 \\sim
F115-F113
 with sigma of 0.01
 C219-F13 \\sim C219-F14 \\sim C219-F15 \\sim C219-F113 \\sim C219-F114 \\sim
C219-F115
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17
\\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim
F101 \\sim F102 \\sim F103 \\sim F104 \\sim F105 \\sim F106 \\sim F107 \\sim
F108 \\sim F109 \\sim F110 \\sim F111 \\sim F112 \\sim F113 \\sim F114 \\sim
F115 \\sim C216 \\sim C316 \\sim C208 \\sim C308 \\sim C307 \\sim C207: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\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(F11) \\sim Ueq,
Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq,
Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F101) \\sim Ueq,
Uanis(F102) \\sim Ueq, Uanis(F103) \\sim Ueq, Uanis(F104) \\sim Ueq,
Uanis(F105) \\sim Ueq, Uanis(F106) \\sim Ueq, Uanis(F107) \\sim Ueq,
Uanis(F108) \\sim Ueq, Uanis(F109) \\sim Ueq, Uanis(F110) \\sim Ueq,
Uanis(F111) \\sim Ueq, Uanis(F112) \\sim Ueq, Uanis(F113) \\sim Ueq,
Uanis(F114) \\sim Ueq, Uanis(F115) \\sim Ueq, Uanis(C216) \\sim Ueq,
Uanis(C316) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(C308) \\sim Ueq,
Uanis(C307) \\sim Ueq, Uanis(C207) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
Uanis(C216) = Uanis(C316)
Uanis(C208) = Uanis(C308)
Uanis(C307) = Uanis(C207)
4. Others
 Sof(F110)=Sof(F111)=Sof(F112)=Sof(C316)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C216)=FVAR(1)
 Sof(F113)=Sof(F114)=Sof(F115)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
 Sof(F104)=Sof(F105)=Sof(F106)=Sof(C308)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(C208)=FVAR(3)
 Sof(F101)=Sof(F102)=Sof(F103)=Sof(C307)=1-FVAR(4)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C207)=FVAR(4)
 Sof(F107)=Sof(F108)=Sof(F109)=1-FVAR(5)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C20(H20), C21(H21), C26(H26), C27(H27),
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230)
;
_shelx_res_checksum              'just to make checkCIF happy'
_shelx_fab_checksum              7492