Hydrogen-bonded adducts between neutral molecules and [Mo(η3-methallyl)(CO)2(HOC(py)3)]+: snapshots of a deprotonation
Morales, Dolores; Pérez, Julio; Martínez-García, Héctor; Puerto, Marcos; del Río, Ignacio; CrystEngComm 13 (2011) 60–; doi:10.1039/c0ce00688b

data_7205499
_publ_section_title
;
 Hydrogen-bonded adducts between neutral molecules and
 [Mo(\h3-methallyl)(CO)2(HOC(py)3)]+: snapshots of a deprotonation
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              60
_journal_paper_doi               10.1039/c0ce00688b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety
'C32 H12 B F24, C22 H20 Mo N3 O3, C6 H12 N2 O, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H48 B Cl4 F24 Mo N5 O4'
_chemical_formula_weight         1631.60
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.6440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3433(4)
_cell_length_b                   21.3842(4)
_cell_length_c                   16.9253(3)
_cell_measurement_reflns_used    12607
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_volume                     6938.8(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43998
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.635
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         12703
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
[1.00000+-1.00000exp(-60.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+19.2780*P+(0.1362P)^2^+0.0000sin\q/\l]
where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2256
_reflns_number_gt                9998
_reflns_number_total             12703
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0CE00688B.TXT
_cod_data_source_block           1H_DMPU_(mp175)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7205499