Directed Synthesis of Noncentrosymmetric Molybdates
Muller, Eric A.; Cannon, Robert J.; Sarjeant, Amy Narducci; Ok, Kang Min; Halasyamani, P. Shiv; Norquist, Alexander J.; Crystal Growth & Design 5 (2005) 1913–; doi:10.1021/cg050184z

data_4505219
_publ_section_title
;
 Directed Synthesis of Noncentrosymmetric Molybdates
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1913
_journal_paper_doi               10.1021/cg050184z
_journal_volume                  5
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C5 H16 Mo3 N2 O14 S1 '
_chemical_formula_sum            'C5 H16 Mo3 N2 O14 S'
_chemical_formula_weight         648.07
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             04-03-06
_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                   8.5398(6)
_cell_length_b                   10.7500(9)
_cell_length_c                   18.1077(11)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      4
_cell_volume                     1662.3(2)
_computing_cell_refinement       'CrysAlis RED '
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2004)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type
; 
CrysAlis CCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24951
_diffrn_reflns_theta_full        31.279
_diffrn_reflns_theta_max         32.925
_diffrn_reflns_theta_min         3.788
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.429
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    2.589
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.63
_refine_diff_density_min         -1.09
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.08(6)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8768
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.000491
_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: 
 38.1 35.0 42.0 7.28 10.4 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0527
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0524
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                3247
_reflns_number_total             5799
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            cg050184zsi20050426_050831.cif
_cod_data_source_block           X0055
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C5 H16 Mo3 N2 O14 S1 '
_cod_database_code               4505219