Design, synthesis and reactivity of dimolybdenum complex bearing quaterphenylene-bridged pyridine-based PNP-type pincer ligand
Eizawa, Aya; Arashiba, Kazuya; Tanaka, Hiromasa; Konomi, Asuka; Yoshizawa, Kazunari; Nishibayashi, Yoshiaki; Dalton Transactions  (2023) –; doi:10.1039/D3DT02887A

data_7713967
_publ_section_title
;
 Design, synthesis and reactivity of dimolybdenum complex bearing
 quaterphenylene-bridged pyridine-based PNP-type pincer ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02887A
_journal_year                    2023
_chemical_formula_moiety         'C82 H128 I6 Mo2 N2 P4'
_chemical_formula_sum            'C82 H128 I6 Mo2 N2 P4'
_chemical_formula_weight         2219.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-07-06 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.233(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.9320(4)
_cell_length_b                   19.0778(4)
_cell_length_c                   30.6795(8)
_cell_measurement_reflns_used    15572
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.31
_cell_volume                     10126.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.800
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.800
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            49727
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.337
_diffrn_reflns_theta_min         1.589
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.74a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4384.00
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.057
_refine_diff_density_max         2.37
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     433
_refine_ls_number_reflns         13312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1009P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7724
_reflns_number_total             13312
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d3dt02887a3.cif
_cod_data_source_block           xcalibur_CCDC1
_cod_database_code               7713967
_shelx_res_checksum              36275
_shelx_fab_checksum              98381