Crystal structures of <i>trans</i>-acetyldicarbonyl(η^5^-cyclopentadienyl)(1,3,5-triaza-7-phosphaadamantane)molybdenum(II) and <i>trans</i>-acetyldicarbonyl(η^5^-cyclopentadienyl)(3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane)molybdenum(II)
Anstey, Mitchell R.; Bost, John L.; Grumman, Anna S.; Kennedy, Nicholas D.; Whited, Matthew T.; Acta Crystallographica Section E 76 (2020) 547–551; doi:10.1107/S2056989020003679

data_2243323
_publ_section_title
;
 Crystal structures of
 <i>trans</i>-acetyldicarbonyl(\h^5^-cyclopentadienyl)(1,3,5-triaza-7-phosphaadamantane)molybdenum(II)
 and
 <i>trans</i>-acetyldicarbonyl(\h^5^-cyclopentadienyl)(3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane)molybdenum(II)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              547
_journal_page_last               551
_journal_paper_doi               10.1107/S2056989020003679
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'[Mo (C5 H5) (C2 H3 O1) (C9 H16 N3 O2 P) (C O)2]'
_chemical_formula_moiety         'C18 H24 Mo N3 O5 P'
_chemical_formula_sum            'C18 H24 Mo N3 O5 P'
_chemical_formula_weight         489.31
_chemical_name_systematic
<i>trans</i>-Acetyldicarbonyl(\h^5^-cyclopentadienyl)(3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane)molybdenum(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.224(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8674(4)
_cell_length_b                   11.6366(3)
_cell_length_c                   14.4655(5)
_cell_measurement_reflns_used    13952
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      31.0170
_cell_measurement_theta_min      2.4950
_cell_volume                     1990.45(12)
_computing_cell_refinement
;
CrysAlisPro (Rigaku, 2019)
;
_computing_data_collection
;
CrysAlisPro (Rigaku, 2019)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku, 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>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy, Single source at offset/far, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38060
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         2.326
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku, 2019)
;
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0017P)^2^+3.9699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                4075
_reflns_number_total             4726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2775sup1.cif
_cod_data_source_block           2
_cod_database_code               2243323
_shelx_hkl_checksum              83991
_shelx_res_checksum              79983
_cod_database_fobs_code 2243323