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_4332612
_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 H34 Mo8 N4 O27 '
_chemical_formula_sum            'C14 H34 Mo8 N4 O27'
_chemical_formula_weight         1457.95
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7611(8)
_cell_length_b                   16.2554(12)
_cell_length_c                   15.6322(11)
_cell_measurement_reflns_used    10105
_cell_measurement_temperature    110
_cell_measurement_theta_max      10.28546
_cell_measurement_theta_min      0.62258
_cell_volume                     3242.7(4)
_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(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_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       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54098
_diffrn_reflns_theta_full        29.345
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         4.060
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.101
_exptl_absorpt_correction_T_max  0.47
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Multifaceted crystal model (Clark & Reid 1995)
;
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    2.986
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.83
_refine_ls_extinction_coef       83(2)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.8332
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.001293
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 32.2 52.4 34.5 16.0 6.96 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0440
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0426
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3153
_reflns_number_total             4896
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic060558tsup1.cif
_cod_data_source_block           Compound-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 b c n '
_cod_original_formula_sum        ' C14 H34 Mo8 N4 O27 '
_cod_database_code               4332612