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_7056682
_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         'C72 H64 Ca O6 P4, Cl14 Mo6, 2(C2 H3 N)'
_chemical_formula_sum            'C76 H70 Ca Cl14 Mo6 N2 O6 P4'
_chemical_formula_weight         2343.24
_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                 108.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.021(5)
_cell_length_b                   16.305(3)
_cell_length_c                   24.931(5)
_cell_measurement_reflns_used    5765
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.94
_cell_measurement_theta_min      2.50
_cell_volume                     8865(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.959
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            40747
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.7937
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         15414
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                10680
_reflns_number_total             15414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj02858j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        8864(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7056682