Alkaline-earth metal based MOFs with second scale long-lasting phosphor behavior
Briones, David; Leo, Pedro; Cepeda, Javier; Orcajo, Gisela; Calleja, Guillermo; Sanz, Raúl; Rodríguez-Diéguez, Antonio; Martínez, Fernando; CrystEngComm 20 (2018) 4793–; doi:10.1039/C8CE00479J

data_7231092
_publ_section_title
;
 Alkaline-earth metal based MOFs with second scale long-lasting phosphor
 behavior
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4793
_journal_paper_doi               10.1039/C8CE00479J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C63 H51 Ca3 N3 O15, 7 (C3 H7 N O)'
_chemical_formula_sum            'C84 H100 Ca3 N10 O22'
_chemical_formula_weight         1721.97
_chemical_name_systematic
'poly-{[tris(mu7-1,3,5-tris(4-carboxyphenyl)benzene-kO:kO':kO'':kO''':k2O'''',O''''':kO'''':kO''''')bis(mu9-1,3,5-tris(4-carboxyphenyl)benzene-kO:kO:kO':kO'':kO'':kO''':kO'''':kO'''':kO''''')(mu6-1,3,5-tris(4-carboxyphenyl)benzene-kO:kO':kO'':kO''':kO'''':kO''''')nonakis(dimethylformamide)octadecacalcium(II)] heneicosa(dimetylfomramide)}'
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-06-10 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   28.5523(8)
_cell_length_b                   28.5523(8)
_cell_length_c                   28.3085(10)
_cell_measurement_reflns_used    47209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.730
_cell_measurement_theta_min      2.295
_cell_volume                     19986.2(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       \w
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47209
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.730
_diffrn_reflns_theta_min         2.295
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8190
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL shelx     R 3 :h       R = 0.06
CELL   28.5523   28.5523   28.3085     90.00     90.00    120.00
SPGR R3
Q101 0.859 0.901 0.562 !       1.28 eA-3
C102 0.564 0.798 0.617 !       0.76 eA-3
C103 0.648 0.414 0.561 !       0.75 eA-3
C104 0.993 0.012 0.335 !       0.71 eA-3
C105 0.718 0.273 0.220 !       0.71 eA-3
C106 0.390 0.724 0.547 !       0.70 eA-3
Q107 0.437 0.366 0.319 !       0.70 eA-3
C108 0.907 0.975 0.962 !       0.70 eA-3
Q109 0.728 0.311 0.904 !       0.69 eA-3
C110 0.430 0.750 0.634 !       0.69 eA-3
C111 0.789 0.008 0.064 !       0.69 eA-3
Q112 0.868 0.958 0.345 !       0.68 eA-3
C113 0.016 0.889 0.907 !       0.68 eA-3
C114 0.460 0.367 0.344 !       0.68 eA-3
C115 0.920 0.502 0.335 !       0.67 eA-3
Q116 0.672 0.383 0.671 !       0.67 eA-3
C117 0.029 0.633 0.133 !       0.66 eA-3
Q118 0.945 0.603 0.328 !       0.66 eA-3
C119 0.947 0.971 0.232 !       0.66 eA-3
C120 0.172 0.719 0.648 !       0.65 eA-3
Q121 0.947 0.164 0.914 !       0.65 eA-3
C122 0.999 0.999 0.930 !       0.65 eA-3
C123 0.978 0.975 0.256 !       0.63 eA-3
C124 0.642 0.211 0.270 !       0.62 eA-3
Q125 0.813 0.780 0.592 !       0.62 eA-3
C126 0.009 0.897 0.938 !       0.62 eA-3
Q127 0.023 0.866 0.899 !       0.61 eA-3
C128 0.978 0.986 0.898 !       0.61 eA-3
C129 0.290 0.523 0.633 !       0.60 eA-3
C130 0.922 0.008 0.861 !       0.60 eA-3
Q131 0.436 0.364 0.290 !       0.60 eA-3
Q132 0.844 0.976 0.898 !       0.60 eA-3
C133 0.042 0.976 0.264 !       0.60 eA-3
C134 0.687 0.210 0.290 !       0.60 eA-3
Q135 0.501 0.783 0.271 !       0.60 eA-3
C136 0.298 0.664 0.914 !       0.59 eA-3
Q137 0.486 0.945 0.173 !       0.59 eA-3
Q138 0.720 0.484 0.573 !       0.59 eA-3
Q139 0.734 0.900 0.522 !       0.59 eA-3
C140 0.492 0.470 0.375 !       0.59 eA-3
C141 0.891 0.116 0.961 !       0.59 eA-3
Q142 0.467 0.335 0.079 !       0.59 eA-3
Q143 0.922 0.803 0.647 !       0.58 eA-3
C144 0.664 0.329 0.641 !       0.58 eA-3
Q145 0.616 0.961 0.643 !       0.58 eA-3
C146 0.967 0.837 0.964 !       0.58 eA-3
Q147 0.157 0.601 0.986 !       0.58 eA-3
C148 0.720 0.034 0.023 !       0.58 eA-3
Q149 0.220 0.813 0.623 !       0.58 eA-3
Q150 0.468 0.344 0.974 !       0.57 eA-3
C151 0.625 0.331 0.540 !       0.57 eA-3
C152 0.974 0.733 0.026 !       0.57 eA-3
Q153 0.070 0.898 0.336 !       0.57 eA-3
C154 0.773 0.485 0.248 !       0.57 eA-3
Q155 0.030 0.212 0.572 !       0.57 eA-3
Q156 0.290 0.320 0.836 !       0.57 eA-3
C157 0.945 0.077 0.244 !       0.57 eA-3
C158 0.607 0.243 0.540 !       0.57 eA-3
C159 0.960 0.985 0.312 !       0.56 eA-3
Q160 0.936 0.695 0.657 !       0.56 eA-3
Q161 0.627 0.938 0.023 !       0.56 eA-3
C162 0.174 0.218 0.640 !       0.55 eA-3
C163 0.211 0.187 0.033 !       0.55 eA-3
Q164 0.944 0.655 0.111 !       0.55 eA-3
Q165 0.975 0.630 0.500 !       0.55 eA-3
Q166 0.579 0.966 0.392 !       0.55 eA-3
Q167 0.596 0.953 0.672 !       0.55 eA-3
Q168 0.118 0.713 0.140 !       0.55 eA-3
Q169 0.244 0.360 0.312 !       0.55 eA-3
C170 0.836 0.891 0.922 !       0.55 eA-3
C171 0.007 0.781 0.023 !       0.55 eA-3
Q172 0.662 0.383 0.134 !       0.55 eA-3
Q173 0.604 0.960 0.477 !       0.55 eA-3
Q174 0.534 0.158 0.344 !       0.55 eA-3
Q175 0.095 0.773 0.499 !       0.54 eA-3
C176 0.405 0.398 0.375 !       0.54 eA-3
C177 0.322 0.678 0.891 !       0.54 eA-3
C178 0.390 0.366 0.819 !       0.54 eA-3
Q179 0.968 0.853 0.281 !       0.54 eA-3
Q180 0.616 0.054 0.330 !       0.54 eA-3
C181 0.258 0.610 0.982 !       0.54 eA-3
C182 0.735 0.213 0.843 !       0.54 eA-3
Q183 0.944 0.608 0.742 !       0.54 eA-3
C184 0.124 0.149 0.361 !       0.54 eA-3
C185 0.023 0.904 0.969 !       0.53 eA-3
Q186 0.289 0.732 0.689 !       0.53 eA-3
C187 0.758 0.445 0.642 !       0.53 eA-3
Q188 0.842 0.570 0.938 !       0.53 eA-3
Q189 0.678 0.031 0.336 !       0.53 eA-3
C190 0.594 0.330 0.610 !       0.53 eA-3
Q191 0.415 0.617 0.001 !       0.53 eA-3
C192 0.374 0.595 0.579 !       0.52 eA-3
C193 0.953 0.474 0.392 !       0.52 eA-3
C194 0.913 0.563 0.375 !       0.52 eA-3
Q195 0.314 0.345 0.342 !       0.52 eA-3
Q196 0.211 0.267 0.718 !       0.52 eA-3
Q197 0.860 0.946 0.892 !       0.52 eA-3
C198 0.053 0.672 0.148 !       0.52 eA-3
Q199 0.398 0.265 0.015 !       0.52 eA-3
;
_refine_diff_density_max         1.923
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         20969
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                14558
_reflns_number_total             20969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00479j2.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
'Adding full bibliography for 7231092--7231094.cif.'
_cod_original_cell_volume        19986.2(13)
_cod_database_code               7231092
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              14147
_shelx_fab_checksum              33776