Reduction of highly bulky triphenolamine molybdenum nitrido and chloride complexes
Bae, Dae Young; Lee, Gunhee; Lee, Eunsung; Dalton Transactions  (2021) –; doi:10.1039/D1DT02375F

data_7708467
_publ_section_title
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 Reduction of highly bulky triphenolamine molybdenum nitrido and chloride
 complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02375F
_journal_year                    2021
_chemical_formula_moiety         'C132 H168 Cl5 K5 Mo2 N2 O6, 2.5(C5 H12)'
_chemical_formula_sum            'C144.5 H198 Cl5 K5 Mo2 N2 O6'
_chemical_formula_weight         2623.67
_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     dual
_audit_creation_date             2021-09-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-09-23 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                111.84(3)
_cell_angle_beta                 100.76(3)
_cell_angle_gamma                99.58(3)
_cell_formula_units_Z            2
_cell_length_a                   18.820(4)
_cell_length_b                   21.472(4)
_cell_length_c                   23.757(5)
_cell_measurement_reflns_used    41484
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.280
_cell_measurement_theta_min      1.184
_cell_volume                     8457(4)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.660
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.886
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            75919
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        23.328
_diffrn_reflns_theta_max         27.280
_diffrn_reflns_theta_min         1.184
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_description       plate
_exptl_crystal_F_000             2782
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.760
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         41484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2162
_refine_ls_wR_factor_ref         0.2444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21927
_reflns_number_total             41484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02375f2.cif
_cod_data_source_block           p-1
_cod_original_formula_sum        'C144.50 H198 Cl5 K5 Mo2 N2 O6'
_cod_database_code               7708467
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C144) = Uanis(C143) = Uanis(C145) = Uanis(C146) = Uanis(C147)
Uanis(C138) = Uanis(C141) = Uanis(C139) = Uanis(C142) = Uanis(C140)
Uanis(C148) = Uanis(C149) = Uanis(C150) = Uanis(C151) = Uanis(C152)
3. Others
 Fixed Sof: C150(0.5) H15A(0.5) H15B(0.5) C151(0.5) H15C(0.5) H15D(0.5)
 C152(0.5) H15E(0.5) H15F(0.5) H15G(0.5) C149(0.5) H14A(0.5) H14B(0.5)
 C143(0.5) H14F(0.5) H14G(0.5) H14H(0.5) C146(0.5) H14I(0.5) H14J(0.5)
 C145(0.5) H14K(0.5) H14L(0.5) C147(0.5) H14M(0.5) H14N(0.5) H14O(0.5)
 C144(0.5) H14P(0.5) H14Q(0.5) C148(0.5) H14C(0.5) H14D(0.5) H14E(0.5)
 C141(0.5) H14R(0.5) H14S(0.5) C139(0.5) H13U(0.5) H13V(0.5) C142(0.5)
 H14T(0.5) H14U(0.5) H14V(0.5) C140(0.5) H14W(0.5) H14X(0.5) C138(0.5)
 H13W(0.5) H13X(0.5) H13Y(0.5)
4.a Ternary CH refined with riding coordinates:
 C127(H127), C20(H20), C51(H51), C61(H61), C17(H17), C39(H39), C7(H7),
 C105(H105), C86(H86), C130(H130), C80(H80), C102(H102), C83(H83), C36(H36),
 C124(H124), C108(H108), C64(H64), C42(H42)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C57(H57A,H57B), C96(H96A,H96B), C118(H11A,H11B), C33(H33A,
 H33B), C77(H77A,H77B), C135(H13L,H13M), C136(H13N,H13O), C150(H15A,H15B),
 C151(H15C,H15D), C134(H13P,H13Q), C149(H14A,H14B), C146(H14I,H14J), C145(H14K,
 H14L), C144(H14P,H14Q), C141(H14R,H14S), C139(H13U,H13V), C140(H14W,H14X)
4.c Me refined with riding coordinates:
 C137(H13I,H13J,H13K), C152(H15E,H15F,H15G), C143(H14F,H14G,H14H), C133(H13R,
 H13S,H13T), C147(H14M,H14N,H14O), C148(H14C,H14D,H14E), C142(H14T,H14U,H14V),
 C138(H13W,H13X,H13Y)
4.d Aromatic/amide H refined with riding coordinates:
 C112(H112), C79(H79), C68(H68), C59(H59), C28(H28), C6(H6), C76(H76),
 C60(H60), C14(H14), C75(H75), C58(H58), C16(H16), C2(H2), C24(H24), C46(H46),
 C101(H101), C119(H119), C50(H50), C29(H29), C15(H15), C97(H97), C35(H35),
 C74(H74), C123(H123), C30(H30), C90(H90), C120(H120), C98(H98), C121(H121),
 C99(H99)
4.e Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C85(H85A,H85B,
 H85C), C106(H10A,H10B,H10C), C128(H12A,H12B,H12C), C9(H9A,H9B,H9C), C129(H12D,
 H12E,H12F), C19(H19A,H19B,H19C), C104(H10D,H10E,H10F), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C81(H81A,H81B,H81C), C52(H52A,H52B,H52C), C40(H40A,H40B,
 H40C), C131(H13C,H13D,H13E), C41(H41A,H41B,H41C), C125(H12G,H12H,H12I),
 C84(H84A,H84B,H84C), C63(H63A,H63B,H63C), C53(H53A,H53B,H53C), C103(H10G,H10H,
 H10I), C132(H13F,H13G,H13H), C43(H43A,H43B,H43C), C82(H82A,H82B,H82C),
 C87(H87A,H87B,H87C), C65(H65A,H65B,H65C), C107(H10J,H10K,H10L), C88(H88A,H88B,
 H88C), C37(H37A,H37B,H37C), C126(H12J,H12K,H12L), C109(H10M,H10N,H10O),
 C110(H11C,H11D,H11E), C38(H38A,H38B,H38C), C44(H44A,H44B,H44C), C66(H66A,H66B,
 H66C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 153.0 electrons were 
found in a volume of 868.0 A^3 in 1 void. 
This is consistent with the presence of 
2 [n-pentane] per formula unit 
which account for 144.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1517
_shelx_fab_checksum              74186
_olex2_submission_special_instructions 'No special instructions were received'