Urea as 'deus ex machina' in giant molybdenum blue type cluster synthesis: an unusual hybrid compound with perspectives for related nano, supramolecular and extended structures
Müller, Achim; Roy, Soumyajit; Schmidtmann, Marc; Bögge, Hartmut; Chemical Communications  (2002) 2000–2002; doi:10.1039/b205887a

data_7114051
_publ_section_title
;
 Urea as 'deus ex machina' in giant molybdenum blue type cluster
 synthesis: an unusual hybrid compound with perspectives for related nano,
 supramolecular and extended structures
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2000
_journal_page_last               2002
_journal_paper_doi               10.1039/b205887a
_journal_year                    2002
_chemical_formula_sum            'C14 H920 Mo154 N28 O894'
_chemical_formula_weight         30566.54
_chemical_name_systematic        ?
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   33.4470(13)
_cell_length_b                   53.320(2)
_cell_length_c                   27.0643(10)
_cell_measurement_reflns_used    7532
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.31
_cell_volume                     46024(3)
_computing_cell_refinement       'Bruker AXS SAINT'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics
'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Bruker AXS SMART'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            136742
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         0.74
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_F_000             29640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.218
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         49716
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_refine_ls_R_factor_obs          0.0523
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0750P)^2^+850.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1845
_refine_ls_wR_factor_obs         0.1412
_reflns_number_observed          34050
_reflns_number_total             50307
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205887a.txt
_cod_data_source_block           krisna
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0750P)^2^+850.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0750P)^2^+850.0000P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        46024.4(30)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7114051