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_7039012
_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 H40 I Mo N3 P2, C3.995 H9.990 O'
_chemical_formula_sum            'C42.995 H49.99 I Mo N3 O P2'
_chemical_formula_weight         909.64
_chemical_name_common            K6PDIMoI
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   10.9610(4)
_cell_length_b                   11.7192(3)
_cell_length_c                   32.6884(10)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.207
_cell_measurement_theta_min      2.237
_cell_volume                     4199.0(2)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2013.6-2 (Bruker-AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            38146
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.023
_refine_ls_abs_structure_details
;
Flack x determined using 3009 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.040(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7978
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0677P)^2^+7.3512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                7296
_reflns_number_total             7978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00301j2.cif
_cod_data_source_block           K6PDIMoI
_cod_depositor_comments
'Adding full bibliography for 7039012--7039014.cif.'
_cod_original_formula_sum        'C42.995 H49.990 I Mo N3 O P2'
_cod_database_code               7039012
_shelx_res_checksum              12693