Crystal structures of phosphine-supported (η^5^-cyclopentadienyl)molybdenum(II) propionyl complexes
Whited, Matthew T.; Ball, Margaret A.; Block, Alison; Brewster, Benjamin A.; Ferrer, LouLou; Jin-Lee, Helen J.; King, Colby J.; North, Jamie D.; Shelton, Inger L.; Wilson, David G.; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021008008

data_2243895
_publ_section_title
;
 Crystal structures of phosphine-supported
 (\h^5^-cyclopentadienyl)molybdenum(II) propionyl complexes
;
_journal_coeditor_code           JQ2008
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021008008
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Mo (C5 H5) (C3 H5 O) (C18 H15 P) (C O)2]'
_chemical_formula_moiety         'C28 H25 Mo O3 P'
_chemical_formula_sum            'C28 H25 Mo O3 P'
_chemical_formula_weight         536.39
_chemical_name_common            CpMo(CO)2(PPh3)(COEt)
_chemical_name_systematic
Dicarbonyl(\h^5^-cyclopentadienyl)propionyl(triphenylphosphane-\k<i>P</i>)molybdenum(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                113.083(2)
_cell_angle_beta                 99.148(2)
_cell_angle_gamma                99.380(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1719(5)
_cell_length_b                   11.7493(7)
_cell_length_c                   12.6049(7)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    170.(2)
_cell_measurement_theta_max      33.1223
_cell_measurement_theta_min      2.6334
_cell_volume                     1195.14(12)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
<i>BIS</i> (Bruker, 2019)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      170.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed--\c Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Curved Graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            49481
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'sealed tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0220P)^2^+0.6108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                5674
_reflns_number_total             5939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jq2008sup1.cif
_cod_data_source_block           1
_cod_database_code               2243895
_shelx_hkl_checksum              22316
_shelx_res_checksum              62358
_cod_database_fobs_code 2243895