Organic-inorganic hybrid rare earth complexes based on polymolybdates with intrinsic photosensitive properties.
Wang, Yuan; Ma, Pengtao; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4679–4682; doi:10.1039/c4dt02967d

data_7033868
_publ_section_title
;
 Organic-inorganic hybrid rare earth complexes based on polymolybdates
 with intrinsic photosensitive properties.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4679
_journal_page_last               4682
_journal_paper_doi               10.1039/c4dt02967d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C59 H199 Gd2 Mo36 N13 O169'
_chemical_formula_weight         7563.65
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.4280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.1061(13)
_cell_length_b                   18.8800(12)
_cell_length_c                   31.161(2)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.44
_cell_volume                     10361.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            50263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    2.841
_exptl_absorpt_correction_T_max  0.5370
_exptl_absorpt_correction_T_min  0.3549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7272
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
 Highly disordered solvent was located in the structures.
 Reflection contributions from this solvent were removed
 using program SQUEEZE, which determined there to be 511 electrons
 in  1801.3 \%A^3^ removed per unit cell. 
 One piperidin-2-one molecule was confirmed from the difference Fourier maps,
 but Ueq values of its atoms are rather high. The molecule could not be located 
 precisely because one oxygen atom is missed during symmetry operation.  
 Thus, the total number of electrons [511] in the void per unit cell,
 equivalent to about 511/2 = 255.5 per molecule unit,   
 is attributed to the hydrogen atoms of the confirmed water molecules 
 from the difference Fourier maps, one disordered piperidin-2-one molecule and 
 another fourteen disordered water molecules.
 Therefore, some reported items that derive from the molecular formula, 
 (e.g., F(000), density, etc.) are correctted. 
;
_refine_diff_density_max         2.932
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         18236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+46.7062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                14512
_reflns_number_total             18236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02967d3.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7033865--7033874.cif.
;
_cod_original_cell_volume        10360.8(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7033868