Stepwise nucleophilic substitution of manganocene, syntheses and structures of the dimer [CpMn(hpp)]2 and the unusual manganate cage [LiMn(hpp)3]2 (hppH = 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2,a]pyrimidine).
Brinkmann, Christine; García, Felipe; Morey, James V.; McPartlin, Mary; Singh, Sanjay; Wheatley, Andrew E. H.; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003)  (2007) 1570–1572; doi:10.1039/b700409e

data_7005297
_publ_section_title
;
 Stepwise nucleophilic substitution of manganocene, syntheses and
 structures of the dimer [CpMn(hpp)]2 and the unusual manganate cage
 [LiMn(hpp)3]2 (hppH =
 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2,a]pyrimidine).
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1570
_journal_page_last               1572
_journal_paper_doi               10.1039/b700409e
_journal_year                    2007
_chemical_formula_sum            'C42 H72 Li2 Mn2 N18'
_chemical_formula_weight         952.94
_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                 107.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.668(3)
_cell_length_b                   18.026(4)
_cell_length_c                   18.697(4)
_cell_measurement_reflns_used    16469
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     4727.3(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25912
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+4.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                7110
_reflns_number_total             9235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700409e.txt
_cod_data_source_block           mw0603
_cod_original_cell_volume        4727.3(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7005297