A molecular loop with interstitial channels in a chiral environment: exploration of the chemistry of Mo24+ species with chiral and non-chiral dicarboxylate anions
Berry, John F.; Cotton, F. Albert; Ibragimov, Sergey A.; Murillo, Carlos A.; Wang, Xiaoping; Dalton Transactions  (2003) 4297–; doi:10.1039/b310151g

data_7013569
_publ_section_title
;
 A molecular loop with interstitial channels in a chiral environment:
 exploration of the chemistry of Mo24+ species with chiral and
 non-chiral dicarboxylate anions
;
_journal_issue                   22
_journal_name_full               'Dalton Transactions'
_journal_page_first              4297
_journal_paper_doi               10.1039/b310151g
_journal_year                    2003
_chemical_formula_moiety         'C88 H92 Cl8 Mo4 N8 O20'
_chemical_formula_sum            'C88 H92 Cl8 Mo4 N8 O20'
_chemical_formula_weight         2249.06
_chemical_name_common
(Mo2(DaniF)2(p-O2CCH(CH3)OC6H4OCH(CH3)CO2)2,4CH2Cl2
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_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                   13.970(3)
_cell_length_b                   20.450(5)
_cell_length_c                   37.216(5)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      41.6
_cell_measurement_theta_min      18.2
_cell_volume                     10632(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Nonius FAST'
_diffrn_measurement_method       '\w scan'
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            12987
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.8684
_exptl_absorpt_correction_T_min  0.7599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         6212
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.1102
_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^)+(0.0152P)^2^+376.0578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2404
_reflns_number_gt                5010
_reflns_number_total             6212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310151g.txt
_cod_data_source_block           cmpd1
_cod_original_sg_symbol_H-M      I222
_cod_database_code               7013569