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_7205501
_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 H19 Mo N3 O3, C6 H16 N, O'
_chemical_formula_sum            'C60 H47 B F24 Mo N4 O4'
_chemical_formula_weight         1450.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.950(5)
_cell_angle_beta                 73.541(5)
_cell_angle_gamma                86.462(5)
_cell_formula_units_Z            2
_cell_length_a                   12.480(5)
_cell_length_b                   13.029(5)
_cell_length_c                   21.067(5)
_cell_measurement_reflns_used    13972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.0696
_cell_measurement_theta_min      3.4103
_cell_volume                     3265(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26741
_diffrn_reflns_theta_full        74.0196
_diffrn_reflns_theta_max         74.0696
_diffrn_reflns_theta_min         3.4103
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.1154
_exptl_crystal_size_mid          0.0883
_exptl_crystal_size_min          0.0486
_refine_diff_density_max         2.113
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         12702
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1546P)^2^+4.8791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2232
_refine_ls_wR_factor_ref         0.2397
_reflns_number_gt                10240
_reflns_number_total             12702
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0CE00688B.TXT
_cod_data_source_block           1H_TEA_(mp283b)
_cod_database_code               7205501