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_2243322
_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 H2 O1) (C6 H12 N3 P) (C O)2]'
_chemical_formula_moiety         'C15 H20 Mo N3 O3 P'
_chemical_formula_sum            'C15 H20 Mo N3 O3 P'
_chemical_formula_weight         417.25
_chemical_name_systematic
<i>trans</i>-Acetyldicarbonyl(\h^5^-cyclopentadienyl)(1,3,5-triaza-7-phosphaadamantane)molybdenum(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.694(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7919(14)
_cell_length_b                   14.5757(13)
_cell_length_c                   12.1140(12)
_cell_measurement_reflns_used    9370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.542
_cell_measurement_theta_min      3.306
_cell_volume                     1647.2(3)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
SAINT (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_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
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32227
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.558
_diffrn_reflns_theta_min         3.306
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.348
_refine_ls_extinction_coef       0.0040(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0124P)^2^+1.3596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                3379
_reflns_number_total             3785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2775sup1.cif
_cod_data_source_block           1
_cod_database_code               2243322
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.875
_shelx_hkl_checksum              5723
_shelx_res_checksum              72012
_cod_database_fobs_code 2243322