Synthetic Approaches for Noncentrosymmetric Molybdates
Desmond J. Hubbard; Alexander R. Johnston; Hernan Sanchez Casalongue; Amy Narducci Sarjeant; Alexander J. Norquist; Inorganic Chemistry 47 (2008) 8518–8525; doi:10.1021/ic800572g

data_4305591
_publ_section_title
;
Synthetic Approaches for Noncentrosymmetric Molybdates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8518
_journal_page_last               8525
_journal_paper_doi               10.1021/ic800572g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C12 H36 Mo8 N4 O26'
_chemical_formula_sum            'C12 H36 Mo8 N4 O26'
_chemical_formula_weight         1419.95
_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             06-07-17
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 97.862(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9257(13)
_cell_length_b                   15.717(2)
_cell_length_c                   11.9316(17)
_cell_measurement_reflns_used    23115
_cell_measurement_temperature    110
_cell_measurement_theta_max      32
_cell_measurement_theta_min      4
_cell_volume                     1658.1(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32948
_diffrn_reflns_theta_full        29.805
_diffrn_reflns_theta_max         31.707
_diffrn_reflns_theta_min         4.012
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.844
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       93(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.001683
_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: 
 0.235E+04 0.344E+04 0.214E+04 0.154E+04 308. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0633
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0466
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3930
_reflns_number_total             5299
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          2.94(2)
_oxford_structure_analysis_title '6301543 Compound X'
_cod_data_source_file            ic800572g-file002_2.cif
_cod_data_source_block           x0263_compound-2
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4305591