Structure of the Elusive Hydrido(methylcyclopentadienyl)dicarbonylmanganate(I) Anion, [(η5-C5H4Me)Mn(CO)2H]-, as Determined by Single-Crystal X-ray Diffraction
Chatterton, Nicholas P.; Guilera, Gemma; McGrady, G. Sean; Organometallics 23 (2004) 1165–; doi:10.1021/om034293r

data_4076270
_publ_section_title
;
 Structure of the Elusive
 Hydrido(methylcyclopentadienyl)dicarbonylmanganate(I) Anion,
 [(\h5-C5H4Me)Mn(CO)2H]-, as Determined by Single-Crystal X-ray
 Diffraction
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1165
_journal_paper_doi               10.1021/om034293r
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C20 H33 K Mn O8'
_chemical_formula_weight         495.50
_chemical_name_common            mnh18
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.360(11)
_cell_angle_beta                 88.989(11)
_cell_angle_gamma                89.096(15)
_cell_formula_units_Z            4
_cell_length_a                   9.4670(19)
_cell_length_b                   13.707(3)
_cell_length_c                   17.709(5)
_cell_measurement_temperature    133(2)
_cell_volume                     2297.2(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13775
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.15
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.9245
_exptl_absorpt_correction_T_min  0.8568
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         8962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0106P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                6196
_reflns_number_total             8962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034293rsi20031208_111202.cif
_cod_data_source_block           C:\structs\nick\mnh18\MNH18NIC.CIF
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076270