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_7708464
_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         'C68 H91 Mo N3 O3, C4 H10 O'
_chemical_formula_sum            'C72 H101 Mo N3 O4'
_chemical_formula_weight         1168.49
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-10 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.22(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.948(8)
_cell_length_b                   9.4800(19)
_cell_length_c                   36.213(7)
_cell_measurement_reflns_used    89521
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.062
_cell_measurement_theta_min      1.058
_cell_volume                     13537(5)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.848
_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     0.660
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            89521
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        23.328
_diffrn_reflns_theta_max         33.062
_diffrn_reflns_theta_min         1.058
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.752
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00210(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         27164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1170P)^2^+5.7883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22119
_reflns_number_total             27164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02375f2.cif
_cod_data_source_block           c2c
_cod_database_code               7708464
_shelx_shelxl_version_number     2016/4
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C51(H51), C54(H54), C10(H10), C35(H35), C13(H13), C7(H7), C57(H57), C32(H32),
 C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C66(H66A,H66B), C44(H44A,H44B), C71(H71A,H71B), C70(H70A,H70B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C63(H63), C18(H18), C17(H17), C2(H2), C46(H46), C24(H24), C39(H39),
 C50(H50), C41(H41), C6(H6), C62(H62), C61(H61), C40(H40), C28(H28)
2.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C37(H37A,H37B,H37C), C53(H53A,H53B,H53C), C52(H52A,H52B,
 H52C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C8(H8A,H8B,
 H8C), C56(H56A,H56B,H56C), C12(H12A,H12B,H12C), C59(H59A,H59B,H59C), C14(H14A,
 H14B,H14C), C36(H36A,H36B,H36C), C58(H58A,H58B,H58C), C69(H69A,H69B,H69C),
 C72(H72A,H72B,H72C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C67(H67A,H67B,
 H67C), C33(H33A,H33B,H33C), C68(H68A,H68B,H68C), C34(H34A,H34B,H34C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              19262
_shelx_fab_checksum              48200
_olex2_submission_special_instructions 'No special instructions were received'