Isolation of a bis(imino)pyridine molybdenum(i) iodide complex through controlled reduction and interconversion of its reaction products.
Pal, Raja; Cherry, Brian R.; Flores, Marco; Groy, Thomas L.; Trovitch, Ryan J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10024–10033; doi:10.1039/c6dt00301j

data_7039013
_publ_section_title
;
 Isolation of a bis(imino)pyridine molybdenum(i) iodide complex through
 controlled reduction and interconversion of its reaction products.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10024
_journal_page_last               10033
_journal_paper_doi               10.1039/c6dt00301j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C39 H41 I Mo N3 P2'
_chemical_formula_sum            'C39 H41 I Mo N3 P2'
_chemical_formula_weight         836.53
_chemical_name_common            K5PDIMoI
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-01-15 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.343(3)
_cell_length_b                   10.343(3)
_cell_length_c                   33.282(10)
_cell_measurement_reflns_used    4957
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      25.2836
_cell_measurement_theta_min      2.3185
_cell_volume                     3560.4(18)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1306
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            28748
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.39
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.622
_refine_ls_abs_structure_details
;
Flack x determined using 990 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+6.8101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                2759
_reflns_number_total             3312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00301j2.cif
_cod_data_source_block           K5PDIMoI
_cod_depositor_comments
'Adding full bibliography for 7039012--7039014.cif.'
_cod_original_cell_volume        3560.(2)
_cod_database_code               7039013
_shelx_res_checksum              50844