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_7708466
_publ_section_title
;
 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         'C70 H92 Cl Mo N O4'
_chemical_formula_sum            'C70 H92 Cl Mo N O4'
_chemical_formula_weight         1142.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-10 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.74(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.259(4)
_cell_length_b                   16.589(3)
_cell_length_c                   18.108(4)
_cell_measurement_reflns_used    18922
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.005
_cell_measurement_theta_min      1.548
_cell_volume                     6229(2)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.005
_diffrn_reflns_theta_min         1.548
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'brownish violet'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0083(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         18922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1153P)^2^+2.2304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14605
_reflns_number_total             18922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02375f2.cif
_cod_data_source_block           p21c_CCDC1
_cod_database_code               7708466
_shelx_shelxl_version_number     2014/7
_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, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C36)=Sof(H36)=1-FVAR(1)
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38)=FVAR(1)
 Fixed Sof: C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5)
3.a Ternary CH refined with riding coordinates:
 C20(H20), C59(H59), C65(H65), C17(H17), C41(H41), C14(H14), C62(H62),
 C33(H33), C38(H38), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C47(H47A,H47B), C1(H1A,H1B), C69(H69A,H69B), C72(H72A,H72B),
 C71(H71A,H71B), C70(H70A,H70B)
3.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C50(H50), C51(H51), C46(H46), C7(H7), C6(H6), C10(H10), C44(H44),
 C5(H5), C57(H57), C12(H12), C55(H55), C45(H45), C31(H31), C29(H29)
3.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C67(H67A,H67B,
 H67C), C60(H60A,H60B,H60C), C18(H18A,H18B,H18C), C42(H42A,H42B,H42C), C61(H61A,
 H61B,H61C), C19(H19A,H19B,H19C), C37(H37A,H37B,H37C), C37(H37D,H37E,H37F),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C43(H43A,H43B,H43C), C34(H34A,H34B,
 H34C), C15(H15A,H15B,H15C), C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              19801
_olex2_submission_special_instructions 'No special instructions were received'