#------------------------------------------------------------------------------
#$Date: 2019-11-24 07:58:02 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/80/4088015.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4088015
loop_
_publ_author_name
'Buck, Dominik M.'
'Kunz, Doris'
_publ_section_title
;
 Triazine Annelated NHC Featuring Unprecedented Coordination Versatility
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5335
_journal_paper_doi               10.1021/acs.organomet.5b00805
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'2 C57 H66 N18 Rh3, 6 B F4, 3 C2H3N, 15 C2H3N'
_chemical_formula_sum            'C150 H186 B6 F24 N54 Rh6'
_chemical_formula_weight         3883.70
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   20.5293(6)
_cell_length_b                   20.5293(6)
_cell_length_c                   24.4165(10)
_cell_measurement_temperature    100(2)
_cell_volume                     8911.7(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX II Duo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            144684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.780
_diffrn_reflns_theta_min         1.417
_diffrn_source                   'micro x-ray tube'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8252
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             4004
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.072
_platon_squeeze_details
;
The unit cell contains 30 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         2.126
_refine_diff_density_min         -1.860
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7903
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0641P)²+49.4819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5024
_reflns_number_total             7903
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00805_si_004.cif
_cod_data_source_block           mo_db509_0m_sq_s
_cod_original_cell_volume        8911.7(6)
_cod_database_code               4088015
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.41508(2) 0.31310(2) 0.52016(2) 0.03449(15) Uani 1 1 d D . . . .
B1 B 0.6667 0.3333 0.6096(5) 0.032(2) Uani 1 3 d DS T P . .
N1 N 0.5875(2) 0.4099(3) 0.4626(2) 0.0389(12) Uani 1 1 d . . . . .
C9 C 0.5593(3) 0.4672(3) 0.6411(3) 0.0355(13) Uani 1 1 d . . . . .
H9 H 0.5679 0.4886 0.6767 0.043 Uiso 1 1 calc R U . . .
N8 N 0.6894(2) 0.5241(2) 0.6009(2) 0.0333(10) Uani 1 1 d . . . . .
C7 C 0.7388(3) 0.5715(3) 0.6391(3) 0.0375(13) Uani 1 1 d . . . . .
H7 H 0.7275 0.5842 0.6738 0.045 Uiso 1 1 calc R U . . .
C6 C 0.8084(3) 0.5969(3) 0.6164(3) 0.0417(15) Uani 1 1 d . . . . .
H6 H 0.8546 0.6311 0.6337 0.050 Uiso 1 1 calc R U . . .
N5 N 0.8027(2) 0.5663(2) 0.5654(2) 0.0360(11) Uani 1 1 d . . . . .
N4 N 0.6912(2) 0.4815(2) 0.5119(2) 0.0341(11) Uani 1 1 d . . . . .
C3 C 0.7154(3) 0.4763(3) 0.4603(3) 0.0356(13) Uani 1 1 d . . . . .
H3 H 0.7661 0.4990 0.4480 0.043 Uiso 1 1 calc R U . . .
C2 C 0.6529(3) 0.4325(3) 0.4307(3) 0.0391(13) Uani 1 1 d . . . . .
H2 H 0.6528 0.4188 0.3935 0.047 Uiso 1 1 calc R U . . .
N10 N 0.4905(2) 0.4161(2) 0.6174(2) 0.0372(12) Uani 1 1 d . . . . .
C11 C 0.4975(3) 0.3960(3) 0.5663(3) 0.0316(12) Uani 1 1 d . . . . .
F11 F 0.6667 0.3333 0.5524(3) 0.0548(17) Uani 1 3 d DS T P . .
N12 N 0.5743(2) 0.4376(2) 0.5577(2) 0.0322(10) Uani 1 1 d . . . . .
F12 F 0.60057(17) 0.32752(18) 0.62809(17) 0.0472(9) Uani 1 1 d D . . . .
C8A C 0.6103(3) 0.4792(3) 0.6026(2) 0.0307(12) Uani 1 1 d . . . . .
C4A C 0.7286(3) 0.5217(3) 0.5574(2) 0.0301(12) Uani 1 1 d . . . . .
C27 C 0.2820(3) 0.3332(3) 0.4890(4) 0.055(2) Uani 1 1 d . . . . .
H27A H 0.2708 0.3324 0.4495 0.066 Uiso 1 1 calc R U . . .
H27B H 0.2571 0.3570 0.5085 0.066 Uiso 1 1 calc R U . . .
C26 C 0.2492(3) 0.2524(4) 0.5092(4) 0.067(2) Uani 1 1 d . . . . .
H26A H 0.2376 0.2505 0.5487 0.080 Uiso 1 1 calc R U . . .
H26B H 0.2014 0.2200 0.4896 0.080 Uiso 1 1 calc R U . . .
C25 C 0.3018(3) 0.2217(3) 0.5006(4) 0.0496(18) Uani 1 1 d D . . . .
H25 H 0.291(3) 0.191(3) 0.528(2) 0.059 Uiso 1 1 d D U . . .
C24 C 0.3441(3) 0.2303(3) 0.4569(3) 0.0475(17) Uani 1 1 d D . . . .
H24 H 0.360(3) 0.199(3) 0.459(2) 0.057 Uiso 1 1 d D U . . .
C23 C 0.3458(4) 0.2708(4) 0.4045(4) 0.059(2) Uani 1 1 d . . . . .
H23A H 0.2964 0.2674 0.3993 0.071 Uiso 1 1 calc R U . . .
H23B H 0.3543 0.2454 0.3731 0.071 Uiso 1 1 calc R U . . .
C22 C 0.4073(4) 0.3533(3) 0.4051(3) 0.0517(17) Uani 1 1 d . . . . .
H22A H 0.4549 0.3572 0.3924 0.062 Uiso 1 1 calc R U . . .
H22B H 0.3937 0.3812 0.3787 0.062 Uiso 1 1 calc R U . . .
C21 C 0.4203(3) 0.3899(3) 0.4593(3) 0.0398(14) Uani 1 1 d D . . . .
H21 H 0.464(3) 0.430(2) 0.464(2) 0.048 Uiso 1 1 d D U . . .
C20 C 0.3665(3) 0.3807(3) 0.4974(3) 0.0418(15) Uani 1 1 d D . . . .
H20 H 0.380(3) 0.413(3) 0.524(2) 0.050 Uiso 1 1 d D U . . .
C12A C 0.6130(3) 0.4398(3) 0.5097(3) 0.0304(12) Uani 1 1 d . . . . .
C14 C 0.4067(4) 0.4570(5) 0.6611(4) 0.072(2) Uani 1 1 d . . . . .
H14A H 0.4453 0.4900 0.6874 0.107 Uiso 1 1 calc R U . . .
H14B H 0.3568 0.4376 0.6775 0.107 Uiso 1 1 calc R U . . .
H14C H 0.4104 0.4854 0.6279 0.107 Uiso 1 1 calc R U . . .
C13 C 0.4188(3) 0.3904(4) 0.6463(3) 0.0495(16) Uani 1 1 d . . . . .
H13A H 0.4184 0.3638 0.6803 0.059 Uiso 1 1 calc R U . . .
H13B H 0.3768 0.3544 0.6229 0.059 Uiso 1 1 calc R U . . .
B2 B 0.6600(8) 0.6482(7) 0.7500 0.094(4) Uani 1 2 d DS TU P . .
F21 F 0.6467(7) 0.5760(6) 0.7500 0.105(2) Uani 0.787(9) 2 d DS TU P A 1
F22 F 0.7027(6) 0.6844(5) 0.7041(3) 0.105(2) Uani 0.787(9) 1 d D U P A 1
F23 F 0.5950(6) 0.6508(6) 0.7500 0.105(2) Uani 0.787(9) 2 d DS TU P A 1
F21A F 0.6122(18) 0.5775(16) 0.7500 0.105(2) Uani 0.213(9) 2 d DS TU P A 2
F22A F 0.6536(15) 0.6719(16) 0.7027(10) 0.105(2) Uani 0.213(9) 1 d D U P A 2
F23A F 0.7255(16) 0.6534(19) 0.7500 0.105(2) Uani 0.213(9) 2 d DS TU P A 2
B3 B 1.0000 1.0000 0.7500 0.139(13) Uani 1 6 d DS TU P . .
F31A F 0.980(11) 0.998(14) 0.6948(15) 0.12(3) Uani 0.059(8) 1 d D U P B -1
F32A F 0.954(5) 1.017(5) 0.782(3) 0.19(2) Uani 0.18(2) 1 d D U P B -1
F31B F 1.017(5) 0.995(6) 0.6949(15) 0.13(2) Uani 0.108(8) 1 d D U P B -2
F32B F 0.9231(10) 0.966(2) 0.756(4) 0.169(17) Uani 0.32(2) 1 d D U P B -2
C31 C 0.7015(7) 0.4470(7) 0.7500 0.071(3) Uani 1 2 d S T P . .
H31A H 0.6802 0.4106 0.7800 0.106 Uiso 0.5 1 calc R U P C -1
H31B H 0.6813 0.4213 0.7150 0.106 Uiso 0.5 1 calc R U P C -1
H31C H 0.6881 0.4862 0.7550 0.106 Uiso 0.5 1 calc R U P C -1
N30 N 0.8453(7) 0.5072(9) 0.7500 0.114(5) Uani 1 2 d S TU P . .
C30 C 0.7835(7) 0.4813(7) 0.7500 0.069(3) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C11 Rh1 N5 87.09(18) . 2_655
C11 Rh1 C21 93.1(2) . .
N5 Rh1 C21 163.2(2) 2_655 .
C11 Rh1 C20 93.6(2) . .
N5 Rh1 C20 159.0(2) 2_655 .
C21 Rh1 C20 37.7(2) . .
C11 Rh1 C25 156.8(3) . .
N5 Rh1 C25 89.2(2) 2_655 .
C21 Rh1 C25 97.0(2) . .
C20 Rh1 C25 82.0(2) . .
C11 Rh1 C24 168.1(2) . .
N5 Rh1 C24 95.0(2) 2_655 .
C21 Rh1 C24 81.5(2) . .
C20 Rh1 C24 88.6(2) . .
C25 Rh1 C24 35.1(3) . .
F12 B1 F12 109.8(5) . 2_655
F12 B1 F12 109.8(5) . 3_665
F12 B1 F12 109.8(5) 2_655 3_665
F12 B1 F11 109.1(5) . .
F12 B1 F11 109.1(5) 2_655 .
F12 B1 F11 109.1(5) 3_665 .
C12A N1 C2 104.0(5) . .
C8A C9 N10 104.5(5) . .
C4A N8 C7 108.7(4) . .
C4A N8 C8A 120.9(5) . .
C7 N8 C8A 130.4(5) . .
N8 C7 C6 104.9(5) . .
C7 C6 N5 111.0(5) . .
C4A N5 C6 104.7(5) . .
C4A N5 Rh1 132.9(4) . 3_665
C6 N5 Rh1 122.2(3) . 3_665
C4A N4 C3 132.3(4) . .
C4A N4 C12A 122.0(5) . .
C3 N4 C12A 105.5(5) . .
C2 C3 N4 106.3(5) . .
C3 C2 N1 110.7(6) . .
C11 N10 C9 113.2(4) . .
C11 N10 C13 125.3(5) . .
C9 N10 C13 121.6(5) . .
N10 C11 N12 102.5(5) . .
N10 C11 Rh1 126.7(4) . .
N12 C11 Rh1 130.2(4) . .
C8A N12 C11 111.0(5) . .
C8A N12 C12A 122.1(4) . .
C11 N12 C12A 126.8(5) . .
C9 C8A N12 108.8(5) . .
C9 C8A N8 133.0(6) . .
N12 C8A N8 118.2(5) . .
N5 C4A N8 110.8(5) . .
N5 C4A N4 129.3(5) . .
N8 C4A N4 119.7(4) . .
C20 C27 C26 113.2(5) . .
C25 C26 C27 112.9(5) . .
C24 C25 C26 127.6(7) . .
C24 C25 Rh1 73.6(3) . .
C26 C25 Rh1 106.6(4) . .
C25 C24 C23 125.8(6) . .
C25 C24 Rh1 71.3(4) . .
C23 C24 Rh1 109.9(4) . .
C24 C23 C22 112.4(6) . .
C21 C22 C23 114.3(6) . .
C20 C21 C22 127.1(6) . .
C20 C21 Rh1 71.8(3) . .
C22 C21 Rh1 108.6(4) . .
C21 C20 C27 125.0(7) . .
C21 C20 Rh1 70.5(3) . .
C27 C20 Rh1 111.8(4) . .
N1 C12A N4 113.5(5) . .
N1 C12A N12 130.0(4) . .
N4 C12A N12 116.6(5) . .
N10 C13 C14 111.6(5) . .
F21A B2 F22A 105.3(11) . .
F21A B2 F22A 105.3(11) . 10_557
F22A B2 F22A 128(3) . 10_557
F21A B2 F23A 105.6(14) . .
F22A B2 F23A 105.5(11) . .
F22A B2 F23A 105.5(11) 10_557 .
F23 B2 F21 112.0(11) . .
F23 B2 F22 110.2(6) . 10_557
F21 B2 F22 108.2(6) . 10_557
F23 B2 F22 110.2(6) . .
F21 B2 F22 108.2(6) . .
F22 B2 F22 107.8(12) 10_557 .
F32B B3 F31B 109(2) . .
F32A B3 F31A 109(2) . .
N30 C30 C31 180.0(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C11 2.038(6) .
Rh1 N5 2.110(4) 2_655
Rh1 C21 2.130(6) .
Rh1 C20 2.147(5) .
Rh1 C25 2.190(6) .
Rh1 C24 2.218(7) .
B1 F12 1.377(5) .
B1 F12 1.378(5) 2_655
B1 F12 1.378(5) 3_665
B1 F11 1.396(14) .
N1 C12A 1.284(8) .
N1 C2 1.415(7) .
C9 C8A 1.336(8) .
C9 N10 1.396(7) .
N8 C4A 1.347(7) .
N8 C7 1.364(7) .
N8 C8A 1.411(6) .
C7 C6 1.369(7) .
C6 N5 1.373(8) .
N5 C4A 1.340(6) .
N5 Rh1 2.110(4) 3_665
N4 C4A 1.369(7) .
N4 C3 1.378(8) .
N4 C12A 1.392(6) .
C3 C2 1.352(8) .
N10 C11 1.342(8) .
N10 C13 1.474(7) .
C11 N12 1.382(6) .
N12 C8A 1.360(7) .
N12 C12A 1.405(7) .
C27 C20 1.520(8) .
C27 C26 1.527(9) .
C26 C25 1.513(9) .
C25 C24 1.330(11) .
C24 C23 1.517(10) .
C23 C22 1.525(9) .
C22 C21 1.479(10) .
C21 C20 1.382(9) .
C14 C13 1.549(9) .
B2 F21A 1.28(3) .
B2 F22A 1.29(2) .
B2 F22A 1.29(2) 10_557
B2 F23A 1.29(3) .
B2 F23 1.363(12) .
B2 F21 1.365(13) .
B2 F22 1.389(10) 10_557
B2 F22 1.389(10) .
B3 F32B 1.378(16) .
B3 F32A 1.379(18) .
B3 F31B 1.41(2) .
B3 F31A 1.40(2) .
C31 C30 1.465(17) .
N30 C30 1.104(16) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.006 -0.004 -0.000 3079 667
