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_7713966
_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 H112 Cl6 Mo2 N2 P4'
_chemical_formula_sum            'C82 H112 Cl6 Mo2 N2 P4'
_chemical_formula_weight         1654.29
_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                 103.0920(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.0001(3)
_cell_length_b                   19.0388(3)
_cell_length_c                   30.0601(5)
_cell_measurement_reflns_used    19153
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.04
_cell_measurement_theta_min      2.20
_cell_volume                     9476.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_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    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.779
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40947
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.995
_diffrn_reflns_theta_min         1.954
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456.00
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.80
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     433
_refine_ls_number_reflns         11772
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0713P)^2^+3.5220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9475
_reflns_number_total             11772
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d3dt02887a3.cif
_cod_data_source_block           xcalibur
_cod_database_code               7713966
_shelx_res_checksum              62411
_shelx_fab_checksum              11676