Assembly of Heterometallic Clusters and Coordination Polymers by Combining Mo−S-Based Clusters with Mn2+
Lin, Ping; Clegg, William; Harrington, Ross W.; Henderson, Richard A.; Fletcher, Ashleigh J.; Bell, Jon; Thomas, K. Mark; Inorganic Chemistry 45 (2006) 4284–4302; doi:10.1021/ic060205u

data_4332302
_publ_section_title
;
 Assembly of Heterometallic Clusters and Coordination Polymers by
 Combining Mo&#x2212;S-Based Clusters with Mn2+
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4284
_journal_page_last               4302
_journal_paper_doi               10.1021/ic060205u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C68 H152 Mn2 Mo8 N4 O18 S24'
_chemical_formula_sum            'C68 H152 Mn2 Mo8 N4 O18 S24'
_chemical_formula_weight         2960.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3218(15)
_cell_length_b                   26.6005(15)
_cell_length_c                   30.184(3)
_cell_measurement_reflns_used    473
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.25
_cell_volume                     11499.1(18)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            71784
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6008
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.57(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         19937
_refine_ls_number_restraints     440
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+22.3846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                16132
_reflns_number_total             19937
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic060205usup6.cif
_cod_data_source_block           6_rah65
_cod_original_cell_volume        11499.3(18)
_cod_database_code               4332302