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_4350709
_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
'C24 H31 Cl2 N5 O Rh, 0.5(C H2 Cl2), C32 H12 B F24'
_chemical_formula_sum            'C56.5 H44 B Cl3 F24 N5 O Rh'
_chemical_formula_weight         1485.03
_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             2014-05-08
_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                100.337(2)
_cell_angle_beta                 97.165(2)
_cell_angle_gamma                113.343(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7330(4)
_cell_length_b                   15.5875(4)
_cell_length_c                   17.0556(5)
_cell_measurement_reflns_used    13916
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.9960
_cell_measurement_theta_min      3.1830
_cell_volume                     2984.88(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0461686000
_diffrn_orient_matrix_UB_12      -0.0083700000
_diffrn_orient_matrix_UB_13      -0.0325805000
_diffrn_orient_matrix_UB_21      0.0185003000
_diffrn_orient_matrix_UB_22      0.0505005000
_diffrn_orient_matrix_UB_23      0.0062821000
_diffrn_orient_matrix_UB_31      0.0372664000
_diffrn_orient_matrix_UB_32      0.0011826000
_diffrn_orient_matrix_UB_33      -0.0278252000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29569
_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         2.941
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1486
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-pentane at 298 K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         12186
_refine_ls_number_restraints     373
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0515P)^2^+4.8901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10478
_reflns_number_total             12186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5024828_si_002.cif
_cod_data_source_block           4b-0063abc14
_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 
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_cod_original_cell_volume        2984.89(16)
_cod_original_formula_sum        'C56.50 H44 B Cl3 F24 N5 O Rh'
_cod_database_code               4350709
_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
2. Restrained distances
 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
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim
C231-F21A
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim
F21A-F19A
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim
C227-F21A
 with sigma of 0.01
 Cl10-C900 \\sim Cl9-C900
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A
\\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 F19A \\sim F20 \\sim
F20A \\sim F21 \\sim F21A \\sim F22 \\sim F23 \\sim F24: within 1.7A with sigma
of 0.007 and sigma for terminal atoms of 0.02
Cl10 \\sim C900 \\sim Cl9: within 2A 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(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6)
\\sim Ueq, Uanis(F6A) \\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(F19A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq,
Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23)
\\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.007 and sigma for terminal
atoms of 0.02
Uanis(C900) \\sim Ueq, Uanis(Cl10) \\sim Ueq, Uanis(Cl9) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl9) = Uanis(Cl10)
Uanis(F19A) = Uanis(F21)
Uanis(F20) = Uanis(F21A)
Uanis(F20A) = Uanis(F19)
Uanis(F6) = Uanis(F5A)
Uanis(F4A) = Uanis(F5)
Uanis(F4) = Uanis(F6A)
4. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Fixed Sof: Cl9(0.5) Cl10(0.5) C900(0.5) H90A(0.5) H90B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), 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), C900(H90A,H90B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C19(H19), C20(H20), C24(H24), C25(H25),
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230)
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