A Tripodal Ligand Constructed from Mesoionic Carbene Donors
Wei-Tsung Lee; Diane A. Dickie; Alejandro J. Metta-Magaña; Jeremy M. Smith; Inorganic Chemistry 52 (2013) 12842–12846; doi:10.1021/ic402311c

data_4336676
_publ_section_title
;
 A Tripodal Ligand Constructed from Mesoionic Carbene Donors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12842
_journal_page_last               12846
_journal_paper_doi               10.1021/ic402311c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C69 H74 B Mn N9 O4.5'
_chemical_formula_weight         1167.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.601(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.4626(17)
_cell_length_b                   27.5033(13)
_cell_length_c                   17.7489(10)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.70
_cell_measurement_theta_min      2.26
_cell_volume                     14841.1(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.1263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            83073
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.340
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_description       plate
_exptl_crystal_F_000             4936
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.473
_exptl_crystal_size_min          0.114
_platon_squeeze_details
;
TITL jsNMSUwtl54_0m in C2/c
CELL   30.4626   27.5033   17.7489     90.00     93.60     90.00
SPGR C2/c
C101 0.501 0.015 0.979 !       5.97 eA-3
C102 0.466 0.022 0.591 !       5.28 eA-3
C103 0.093 0.055 0.787 !       3.75 eA-3
C104 0.614 0.359 0.237 !       3.54 eA-3
C105 0.530 0.040 0.879 !       3.40 eA-3
C106 0.053 0.051 0.547 !       3.33 eA-3
C107 0.577 0.483 0.837 !       3.32 eA-3
C108 0.077 0.983 0.837 !       3.32 eA-3
C109 0.452 0.469 0.575 !       3.28 eA-3
C110 0.594 0.388 0.297 !       3.15 eA-3
C111 0.580 0.406 0.153 !       3.04 eA-3
C112 0.587 0.432 0.266 !       3.03 eA-3
C113 0.459 0.454 0.437 !       2.85 eA-3
C114 0.915 0.033 0.636 !       2.59 eA-3
C115 0.610 0.373 0.185 !       2.52 eA-3
C116 0.463 0.498 0.219 !       2.44 eA-3
C117 0.423 0.466 0.530 !       2.42 eA-3
C118 0.435 0.494 0.639 !       2.38 eA-3
C119 0.070 0.083 0.574 !       2.34 eA-3
C120 0.926 0.084 0.865 !       2.32 eA-3
C121 0.921 0.114 0.815 !       2.21 eA-3
C122 0.929 0.076 0.728 !       2.20 eA-3
C123 0.039 0.015 0.292 !       2.00 eA-3
C124 0.098 0.162 0.765 !       1.91 eA-3
C125 0.080 0.141 0.712 !       1.90 eA-3
C126 0.430 0.419 0.256 !       1.89 eA-3
C127 0.576 0.396 0.213 !       1.85 eA-3
C128 0.542 0.405 0.068 !       1.80 eA-3
C129 0.070 0.043 0.827 !       1.79 eA-3
C130 0.498 0.004 0.079 !       1.73 eA-3
C131 0.024 0.012 0.766 !       1.68 eA-3
C132 0.070 0.056 0.433 !       1.55 eA-3
C133 0.939 0.492 0.051 !       1.47 eA-3
C134 0.962 0.087 0.879 !       1.46 eA-3
C135 0.899 0.095 0.828 !       1.43 eA-3
C136 0.946 0.111 0.918 !       1.40 eA-3
C137 0.443 0.391 0.229 !       1.37 eA-3
C138 0.074 0.486 0.405 !       1.35 eA-3
C139 0.966 0.466 0.593 !       1.32 eA-3
C140 0.954 0.055 0.861 !       1.32 eA-3
C141 0.483 0.477 0.439 !       1.31 eA-3
C142 0.460 0.031 0.524 !       1.31 eA-3
C143 0.968 0.069 0.682 !       1.31 eA-3
C144 0.975 0.076 0.958 !       1.30 eA-3
C145 0.991 0.429 0.094 !       1.29 eA-3
C146 0.954 0.016 0.926 !       1.28 eA-3
C147 0.139 0.166 0.764 !       1.26 eA-3
C148 0.487 0.056 0.518 !       1.25 eA-3
C149 0.598 0.484 0.323 !       1.25 eA-3
C150 0.966 0.020 0.003 !       1.23 eA-3
C151 0.108 0.023 0.357 !       1.23 eA-3
C152 0.944 0.118 0.755 !       1.23 eA-3
C153 0.928 0.016 0.707 !       1.21 eA-3
C154 0.548 0.479 0.027 !       1.21 eA-3
C155 0.431 0.452 0.213 !       1.20 eA-3
C156 0.100 0.149 0.814 !       1.19 eA-3
Q157 0.737 0.353 0.281 !       1.18 eA-3
C158 0.601 0.456 0.815 !       1.17 eA-3
C159 0.930 0.120 0.710 !       1.16 eA-3
C160 0.517 0.489 0.469 !       1.16 eA-3
C161 0.040 0.058 0.782 !       1.15 eA-3
C162 0.540 0.558 0.782 !       1.15 eA-3
C163 0.397 0.354 0.373 !       1.14 eA-3
C164 0.104 0.188 0.700 !       1.14 eA-3
C165 0.977 0.109 0.925 !       1.12 eA-3
Q166 0.463 0.336 0.283 !       1.11 eA-3
C167 0.024 0.493 0.325 !       1.11 eA-3
C168 0.952 0.021 0.671 !       1.11 eA-3
C169 0.445 0.495 0.108 !       1.11 eA-3
C170 0.051 0.493 0.874 !       1.09 eA-3
Q171 0.653 0.358 0.205 !       1.09 eA-3
Q172 0.930 0.469 0.566 !       1.08 eA-3
C173 0.449 0.405 0.304 !       1.06 eA-3
C174 0.088 0.042 0.564 !       1.06 eA-3
C175 0.573 0.617 0.808 !       1.05 eA-3
C176 0.977 0.477 0.954 !       1.05 eA-3
C177 0.460 0.419 0.223 !       1.03 eA-3
C178 0.984 0.458 0.537 !       1.02 eA-3
C179 0.106 0.224 0.707 !       1.02 eA-3
C180 0.437 0.363 0.200 !       1.02 eA-3
C181 0.994 0.448 0.988 !       1.01 eA-3
C182 0.997 0.462 0.311 !       1.01 eA-3
C183 0.135 0.115 0.738 !       1.01 eA-3
C184 0.962 0.490 0.482 !       1.01 eA-3
C185 0.498 0.029 0.876 !       1.01 eA-3
C186 0.399 0.334 0.348 !       1.01 eA-3
C187 0.026 0.024 0.405 !       1.00 eA-3
C188 0.993 0.044 0.968 !       1.00 eA-3
C189 0.461 0.044 0.732 !       1.00 eA-3
C190 0.471 0.485 0.659 !       0.99 eA-3
C191 1.003 0.406 0.390 !       0.99 eA-3
C192 0.046 0.077 0.894 !       0.97 eA-3
C193 0.959 0.436 0.966 !       0.97 eA-3
C194 0.506 0.073 0.875 !       0.97 eA-3
Q195 0.037 0.486 0.063 !       0.97 eA-3
C196 0.923 0.017 0.970 !       0.97 eA-3
C197 0.021 0.478 0.878 !       0.96 eA-3
C198 0.647 0.372 0.236 !       0.96 eA-3
C199 0.967 0.058 0.233 !       0.95 eA-3
;
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         14082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0819P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7566
_reflns_number_total             14082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402311c_si_001_2.cif
_cod_data_source_block           jsnmsuwtl54_0m_a_sq_s
_cod_depositor_comments
;

2021-04-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C138 H148 B2 Mn2 N18 O9'
_cod_original_formula_weight         2334.24
_cod_original_formula_units_Z            4
_cod_database_code               4336676
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2013-2
_shelx_res_checksum              93280
_shelx_fab_checksum              58251