Two molybdenum pentacarbonyl complexes with electroneutral phosphane ligands: [bis(morpholin-4-yl)(pentafluoroethyl)phosphane-κ<i>P</i>]pentacarbonylmolybdenum(0) and pentacarbonyl[(pentafluoroethyl)bis(piperidin-1-yl)phosphane-κ<i>P</i>]molybdenum(0)
Petrochko, Natalia G.; Peters, R. Gregory; Baughman, Russell G.; Acta Crystallographica Section C 70 (2014) 508–511; doi:10.1107/S2053229614007165

data_2019530
_publ_section_title
;
 Two molybdenum pentacarbonyl complexes with electroneutral phosphane
 ligands:
 [bis(morpholin-4-yl)(pentafluoroethyl)phosphane-\k<i>P</i>]pentacarbonylmolybdenum(0)
 and
 pentacarbonyl[(pentafluoroethyl)bis(piperidin-1-yl)phosphane-\k<i>P</i>]molybdenum(0)
;
_journal_coeditor_code           EG3158
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              508
_journal_page_last               511
_journal_paper_doi               10.1107/S2053229614007165
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Mo (C12 H20 F5 N2 P) (C O)5]'
_chemical_formula_moiety         'C17 H20 F5 Mo N2 O5 P'
_chemical_formula_sum            'C17 H20 F5 Mo N2 O5 P'
_chemical_formula_weight         554.26
_chemical_name_systematic
Pentacarbonyl[(pentafluoroethyl)bis(piperidin-1-yl)phosphane-\k<i>P</i>]molybdenum(0)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.110(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4472(3)
_cell_length_b                   15.8563(6)
_cell_length_c                   14.0067(6)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      10.05
_cell_volume                     2240.05(15)
_computing_cell_refinement       'XSCANS (Bruker, 1996)'
_computing_data_collection       'XSCANS (Bruker, 1996)'
_computing_data_reduction        'XSCANS (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL/PC (Sheldrick, 2008) and SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6372
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XSHELL; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'parallelepiped cut from larger block'
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          .40
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.382
_refine_ls_extinction_coef       0.0122(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.7523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                4324
_reflns_number_total             5120
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3158sup1.cif
_cod_data_source_block           2a
_cod_original_cell_volume        2240.05(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019530
_cod_database_fobs_code          2019530