Tetracarbonyl[<i>N</i>-(diphenylphosphanyl-κ<i>P</i>)-<i>N</i>,<i>N</i>'-diisopropyl-<i>P</i>-phenylphosphorus diamide-κ<i>P</i>]molybdenum(0) with an unknown solvent
Höhne, Martha; Gongoll, Marc; Spannenberg, Anke; Müller, Bernd H.; Peulecke, Normen; Rosenthal, Uwe; IUCrData 3 (2018) x180846–; doi:10.1107/S2414314618008465

data_1549606
_publ_section_title
;
 Tetracarbonyl[<i>N</i>-(diphenylphosphanyl-\k<i>P</i>)-<i>N</i>,<i>N</i>'-diisopropyl-<i>P</i>-phenylphosphorus
 diamide-\k<i>P</i>]molybdenum(0) with an unknown solvent
;
_journal_coeditor_code           RZ4024
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x180846
_journal_paper_doi               10.1107/S2414314618008465
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          '[Mo (C24 H30 N2 P2) (C O)4]'
_chemical_formula_moiety         'C28 H30 Mo N2 O4 P2'
_chemical_formula_sum            'C28 H30 Mo N2 O4 P2'
_chemical_formula_weight         616.42
_chemical_name_systematic
'Tetracarbonyl[<i>N</i>-(diphenylphosphanyl-\k<i>P</i>)-<i>N</i>,<i>N</i>'-diisopropyl-<i>P</i>-phenylphosphorus diamide-\k<i>P</i>]molybdenum(0)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.634(3)
_cell_length_b                   17.716(4)
_cell_length_c                   21.661(4)
_cell_measurement_reflns_used    11600
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      1.84
_cell_volume                     5999(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2005)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2005)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2005)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            95647
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.880
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2005)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_platon_squeeze_details
;
Contributions of solvent molecules were removed from the
diffraction data with PLATON / SQUEEZE (Spek, 2015).
;
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6886
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                5657
_reflns_number_total             6886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz4024sup1.cif
_cod_data_source_block           I
_cod_database_code               1549606
_shelx_hkl_checksum              32871
_shelx_res_checksum              63651
_cod_database_fobs_code 1549606