Mixed-solvothermal synthesis, structures, luminescent and surface photovoltage properties of four new transition metal diphosphonates with a 3D supramolecular structure
Tian, Hui; Zhu, Yan-Yu; Sun, Zhen-Gang; Tong, Fei; Zhu, Jiang; Chu, Wei; Sun, Shou-Hui; Zheng, Ming-Jing; New Journal of Chemistry 37 (2013) 212–; doi:10.1039/c2nj40737j

data_7053100
_publ_section_title
;
 Mixed-solvothermal synthesis, structures, luminescent and surface
 photovoltage properties of four new transition metal diphosphonates with
 a 3D supramolecular structure
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              212
_journal_paper_doi               10.1039/c2nj40737j
_journal_volume                  37
_journal_year                    2013
_chemical_formula_sum            'C15 H58 N4 Ni O24 P6'
_chemical_formula_weight         923.18
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   16.6093(7)
_cell_length_b                   16.6093(7)
_cell_length_c                   51.213(4)
_cell_measurement_reflns_used    5264
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.39
_cell_volume                     12235.3(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Smart Apex II CCD'
_diffrn_measurement_method       'omega 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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            21856
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.7620
_exptl_absorpt_correction_T_min  0.7179
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5832
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.739
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2832
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+70.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1666
_reflns_number_gt                2190
_reflns_number_total             2832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40737j.txt
_cod_data_source_block           0924f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        12235.4(12)
_cod_original_sg_symbol_H-M      'R-3c '
_cod_database_code               7053100