Syntheses, structural characterization and photophysical properties of two series of rare-earth-isonicotinic-acid containing Waugh-type manganomolybdates
Gong, Peijun; Li, Yanyan; Zhai, Cuiping; Luo, Jie; Tian, Xuemeng; Chen, Lijuan; Zhao, Junwei; CrystEngComm 19 (2017) 834–; doi:10.1039/C6CE02428A

data_7227300
_publ_section_title
;
 Syntheses, structural characterization and photophysical properties of
 two series of rare-earth-isonicotinic-acid containing Waugh-type
 manganomolybdates
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              834
_journal_paper_doi               10.1039/C6CE02428A
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C24 H18 Mn2 Mo18 N4 Nd2 O76, 12(O), 8(N)'
_chemical_formula_sum            'C24 H82 Mn2 Mo18 N12 Nd2 O88'
_chemical_formula_weight         4072.30
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-16 deposited with the CCDC.
2016-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                72.8930(10)
_cell_angle_beta                 82.0370(10)
_cell_angle_gamma                89.3050(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4141(4)
_cell_length_b                   12.6941(5)
_cell_length_c                   19.1513(9)
_cell_measurement_reflns_used    5145
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.309
_cell_measurement_theta_min      2.248
_cell_volume                     2395.32(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12304
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.710
_exptl_absorpt_correction_T_max  0.7080
_exptl_absorpt_correction_T_min  0.4958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.288
_refine_diff_density_min         -3.119
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.00019(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         8326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0523P)^2^+1.9231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                6865
_reflns_number_total             8326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce02428a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7227298--7227310.cif.'
_cod_database_code               7227300
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1W-O6W_$2
 2.8 with sigma of 0.01
3. Others
 Fixed Uiso: O6W(0.0945) O7W(0.09508)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C7(H7A), C8(H8A), C9(H9A), C10(H10A)
4.b Tetrahedral OH refined with riding coordinates:
 O33(H33A)
;
_olex2_submission_special_instructions 'No special instructions were received'