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_7708465
_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         'C68 H94 Mo N3 O3'
_chemical_formula_sum            'C68 H94 Mo N3 O3'
_chemical_formula_weight         1097.40
_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   mixed
_atom_sites_solution_primary     dual
_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                 103.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.558(4)
_cell_length_b                   16.423(3)
_cell_length_c                   18.064(4)
_cell_measurement_reflns_used    10192
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.333
_cell_measurement_theta_min      2.268
_cell_volume                     6228(2)
_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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27742
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        24.333
_diffrn_reflns_theta_max         24.333
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0548P)^2^+8.8397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9869
_reflns_number_total             10192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02375f2.cif
_cod_data_source_block           p21c
_cod_database_code               7708465
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H36A)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=1-FVAR(1)
 Sof(H36)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N3(H3), C11(H11), C17(H17), C62(H62), C56(H56), C14(H14), C40(H40), C33(H33),
 C36(H36), C36(H36A), C59(H59)
3.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C23(H23A,H23B), C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C67(H67), C21(H21), C20(H20), C22(H22), C7(H7), C45(H45), C66(H66), C65(H65),
 C54(H54), C43(H43), C44(H44), C29(H29), C9(H9), C52(H52), C31(H31)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C57(H57A,H57B,
 H57C), C13(H13A,H13B,H13C), C63(H63A,H63B,H63C), C69(H69A,H69B,H69C), C58(H58A,
 H58B,H58C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C37(H37A,H37B,H37C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C64(H64A,H64B,H64C), C68(H68A,H68B,
 H68C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C), C38(H38A,
 H38B,H38C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              34564
_olex2_submission_special_instructions 'No special instructions were received'