Directed Synthesis of Noncentrosymmetric Molybdates Using Composition Space Analysis
Veltman, Thomas R.; Stover, Adam K.; Narducci Sarjeant, Amy; Ok, Kang Min; Halasyamani, P. Shiv; Norquist, Alexander J.; Inorganic Chemistry 45 (2006) 5529–5537; doi:10.1021/ic060558t

data_4332613
_publ_section_title
;
 Directed Synthesis of Noncentrosymmetric Molybdates Using Composition
 Space Analysis
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5529
_journal_page_last               5537
_journal_paper_doi               10.1021/ic060558t
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C14 H40 Mo8 N4 O30 '
_chemical_formula_sum            'C14 H40 Mo8 N4 O30'
_chemical_formula_weight         1512.00
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-13-01
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 94.684(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9547(3)
_cell_length_b                   11.0404(5)
_cell_length_c                   20.6373(7)
_cell_measurement_reflns_used    15455
_cell_measurement_temperature    110
_cell_measurement_theta_max      10.15080
_cell_measurement_theta_min      0.61880
_cell_volume                     1806.38(12)
_computing_cell_refinement       'CrysAlis RED '
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2004)'
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type
; 
CrysAlis CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32095
_diffrn_reflns_theta_full        29.620
_diffrn_reflns_theta_max         34.847
_diffrn_reflns_theta_min         3.843
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Multifaceted crystal model (Clark & Reid 1995)
;
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    2.780
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.76
_refine_ls_extinction_coef       9.7(15)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.9495
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.002993
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ 
 Method = SHELXL 97 (Sheldrick, 1997) 
 W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] 
 P(i) are: 
 0.238E-01 0.00 0.00 0.00 0.00 0.333 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0483
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0440
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                5181
_reflns_number_total             7288
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic060558tsup1.cif
_cod_data_source_block           Compound-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C14 H40 Mo8 N4 O30 '
_cod_database_code               4332613