Luminescent Coordination Polymers Based on Ca2+ and Octahedral Cluster Anions [{M6Cli8}Cla6]2– (M = Mo, W): Synthesis and Thermal Stability Studies
Evtushok, Darya V.; Vorotnikova, Natalya A.; Logvinenko, Vladimir A.; Smolentsev, Anton I.; Brylev, Konstantin; Plyusnin, Pavel E.; Pishchur, Denis P.; Kitamura, N.; Mironov, Yuri V.; Solovieva, Anastasiya O.; Efremova, Olga A.; Shestopalov, Michael A.; New J. Chem. 41 (2017) 14855–14861; doi:10.1039/C7NJ02858J

data_7056683
_publ_section_title
;
 Luminescent Coordination Polymers Based on Ca2+ and Octahedral Cluster
 Anions [{M6Cli8}Cla6]2-- (M = Mo, W): Synthesis and Thermal Stability
 Studies
;
_journal_issue                   24
_journal_name_full               'New J. Chem.'
_journal_page_first              14855
_journal_page_last               14861
_journal_paper_doi               10.1039/C7NJ02858J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'Cl14 W6, C72 H60 Ca O4 P4'
_chemical_formula_sum            'C72 H60 Ca Cl14 O4 P4 W6'
_chemical_formula_weight         2752.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-07-31 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.2120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3726(10)
_cell_length_b                   14.1362(6)
_cell_length_c                   24.2685(11)
_cell_measurement_reflns_used    6008
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.73
_cell_volume                     7999.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26998
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.251
_exptl_absorpt_correction_T_max  0.3375
_exptl_absorpt_correction_T_min  0.2591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.522
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         9037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                6061
_reflns_number_total             9037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj02858j2.cif
_cod_data_source_block           1_CCDC1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7056683