Supramolecular structure of {C6H2[CH2OCH2C(pz)3]4[Mn(CO)3]4}(BF4)4 based on tetrametallic organometallic building blocks constructed from a multitopic tris(pyrazolyl)methane ligand
Daniel L. Reger; Radu F. Semeniuc; Mark D. Smith; J. Chem. Soc., Dalton Trans.  (2002) 476–477; doi:10.1039/b110095e

data_7011282
_publ_section_title
;
 Supramolecular structure of {C6H2[CH2OCH2C(pz)3]4[Mn(CO)3]4}(BF4)4
 based on tetrametallic organometallic building blocks constructed from
 a multitopic tris(pyrazolyl)methane ligand
;
_journal_issue                   4
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              476
_journal_page_last               477
_journal_paper_doi               10.1039/b110095e
_journal_year                    2002
_chemical_formula_moiety
; 
{C54H54N24O4[Mn(CO)3]4} {BF4}4 (CH3CN)6 (Et2O)2 
;
_chemical_formula_sum            'C86 H92 B4 F16 Mn4 N30 O18'
_chemical_formula_weight         2400.90
_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                 99.538(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8441(9)
_cell_length_b                   17.6246(13)
_cell_length_c                   25.6874(19)
_cell_measurement_reflns_used    6214
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.310
_cell_measurement_theta_min      2.311
_cell_volume                     5288.1(7)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34997
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         10830
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.1418P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2164
_reflns_number_gt                7517
_reflns_number_total             10830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110095e.txt
_cod_data_source_block           mn1245s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7011282