Preparation and reactivity of molybdenum complexes bearing pyrrole-based PNP-type pincer ligand.
Tanabe, Yoshiaki; Sekiguchi, Yoshiya; Tanaka, Hiromasa; Konomi, Asuka; Yoshizawa, Kazunari; Kuriyama, Shogo; Nishibayashi, Yoshiaki; Chemical communications (Cambridge, England) 56 (2020) 6933–6936; doi:10.1039/d0cc02852e

data_7126612
_publ_section_title
;
 Preparation and reactivity of molybdenum complexes bearing pyrrole-based
 PNP-type pincer ligand.
;
_journal_issue                   51
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6933
_journal_page_last               6936
_journal_paper_doi               10.1039/d0cc02852e
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52 H100 K Mo2 N8 O2 P4'
_chemical_formula_sum            'C52 H100 K Mo2 N8 O2 P4'
_chemical_formula_weight         1224.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-05-01 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.2771(4)
_cell_length_b                   18.0042(4)
_cell_length_c                   20.8139(4)
_cell_measurement_reflns_used    36922
_cell_measurement_temperature    198
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      1.95
_cell_volume                     6099.6(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, 2018)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.1586
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44031
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.950
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             2588.00
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.58
_refine_ls_abs_structure_details
;
 No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     647
_refine_ls_number_reflns         13167
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+-0.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                9002
_reflns_number_total             13167
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0cc02852e2.cif
_cod_data_source_block           C44H84K1Mo2N8P4-2C4H8O
_cod_depositor_comments
'Adding full bibliography for 7126610--7126613.cif.'
_cod_database_code               7126612
_shelx_res_checksum              89318
_shelx_hkl_checksum              83989