Novel Linear Transition Metal Clusters of a Heptadentate Bis-β-diketone Ligand
Guillem Aromí; Patrick Gamez; J. Krzystek; Huub Kooijman; Anthony L. Spek; Elizabeth J. MacLean; Simon J. Teat; Harriott Nowell; Inorganic Chemistry 46 (2007) 2519–2529; doi:10.1021/ic062075v

data_4307594
_publ_contact_author_address
;   Bijvoet Center for Biomolecular Research
    Crystal and Structural Chemistry
    Utrecht University
    Padualaan 8
    3584 CH Utrecht
    The Netherlands
;
_publ_contact_author_email       h.kooijman@chem.uu.nl
_publ_contact_author_fax         '+31 30 2533940'
_publ_contact_author_name        '   Dr. H. Kooijman'
_publ_contact_author_phone       '+31 30 2532533'
_publ_section_title
;
Novel Linear Transition Metal Clusters of a Heptadentate Bis-\b-diketone
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2519
_journal_page_last               2529
_journal_paper_doi               10.1021/ic062075v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C85.5 H66 Mn3 N7.5 O14.25'
_chemical_formula_weight         1591.28
_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                98.608(2)
_cell_angle_beta                 94.671(2)
_cell_angle_gamma                91.647(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5020(3)
_cell_length_b                   17.7237(5)
_cell_length_c                   19.9453(5)
_cell_measurement_reflns_used    5962
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.38
_cell_volume                     3655.34(17)
_computing_cell_refinement       'Bruker SAINT v7.06a'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT v7.06a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'SIR2002 run through WINGX'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6894
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42477
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         1.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1641
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.936
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         21645
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0750P)^2^+2.4753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                16334
_reflns_number_total             21645
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic062075vsi20061030_124021_1.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C85.50 H66 Mn3 N7.50 O14.25'
_cod_database_code               4307594