Photoluminescent calcium azolium carboxylates with diversified calcium coordination geometry and thermal stability.
Suresh, Paladugu; Naga Babu, Chatla; Sampath, Natarajan; Prabusankar, Ganesan; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7338–7346; doi:10.1039/c5dt00480b

data_7034573
_publ_section_title
;
 Photoluminescent calcium azolium carboxylates with diversified calcium
 coordination geometry and thermal stability.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7338
_journal_page_last               7346
_journal_paper_doi               10.1039/c5dt00480b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C78 H88 Ca2.5 N12 O20, 6(Br)'
_chemical_formula_sum            'C78 H88 Br6 Ca2.5 N12 O20'
_chemical_formula_weight         2093.26
_chemical_name_systematic        6
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-02 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                89.717(3)
_cell_angle_beta                 74.471(4)
_cell_angle_gamma                75.245(4)
_cell_formula_units_Z            2
_cell_length_a                   14.3416(7)
_cell_length_b                   20.7798(8)
_cell_length_c                   21.1629(8)
_cell_measurement_reflns_used    22056
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.85
_cell_measurement_theta_min      3.20
_cell_volume                     5862.7(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22056
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.853
_diffrn_reflns_theta_min         3.198
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         22056
_exptl_absorpt_coefficient_mu    3.898
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       Block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Approximately 30% of the unit cell volume comprises a 
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 114 electrons per unit cell.
 

TITL exp_2409  P -1         R = 0.11
CELL   14.3416   20.7798   21.1629     89.72     74.47     75.25
SPGR P-1
Q101 1.000 0.500 0.500 !       3.79 eA-3
Q102 0.579 0.466 0.219 !       2.90 eA-3
Q103 0.764 0.590 0.727 !       2.78 eA-3
Q104 0.515 0.976 0.736 !       2.56 eA-3
Q105 0.876 0.505 0.751 !       2.36 eA-3
Q106 0.499 0.262 0.260 !       2.18 eA-3
Q107 0.113 0.422 0.199 !       2.15 eA-3
Q108 0.279 0.476 0.259 !       2.04 eA-3
Q109 0.702 0.544 0.730 !       1.91 eA-3
Q110 0.285 0.250 0.530 !       1.78 eA-3
Q111 0.160 0.340 0.261 !       1.70 eA-3
Q112 0.015 0.927 0.956 !       1.56 eA-3
Q113 0.656 0.217 0.987 !       1.39 eA-3
Q114 0.782 0.232 0.103 !       1.30 eA-3
Q115 0.202 0.886 0.770 !       1.09 eA-3
Q116 0.751 0.393 0.619 !       1.02 eA-3
Q117 0.841 0.638 0.605 !       1.01 eA-3
Q118 0.722 0.646 0.643 !       0.97 eA-3
Q119 0.173 0.380 0.282 !       0.95 eA-3
Q120 0.185 0.427 0.244 !       0.95 eA-3
Q121 0.405 0.323 0.699 !       0.95 eA-3
Q122 0.751 0.651 0.621 !       0.95 eA-3
Q123 0.122 0.333 0.667 !       0.93 eA-3
Q124 0.840 0.876 0.120 !       0.93 eA-3
Q125 0.104 0.838 0.185 !       0.93 eA-3
Q126 0.282 0.393 0.324 !       0.91 eA-3
Q127 0.596 0.745 0.298 !       0.90 eA-3
Q128 0.643 0.268 0.407 !       0.90 eA-3
Q129 0.111 0.927 0.018 !       0.90 eA-3
Q130 0.562 0.601 0.530 !       0.90 eA-3
Q131 0.388 0.045 0.110 !       0.88 eA-3
Q132 0.641 0.255 0.572 !       0.84 eA-3
Q133 0.920 0.183 0.829 !       0.84 eA-3
Q134 0.594 0.266 0.796 !       0.82 eA-3
C135 0.064 0.024 0.368 !       0.82 eA-3
Q136 0.546 0.209 0.637 !       0.81 eA-3
Q137 0.783 0.203 0.758 !       0.81 eA-3
C138 0.205 0.631 0.830 !       0.81 eA-3
Q139 0.592 0.123 0.624 !       0.79 eA-3
Q140 0.551 0.657 0.797 !       0.79 eA-3
Q141 0.247 0.300 0.233 !       0.79 eA-3
Q142 0.348 0.264 0.737 !       0.76 eA-3
Q143 0.309 0.422 0.312 !       0.76 eA-3
Q144 0.451 0.083 0.033 !       0.75 eA-3
C145 0.833 0.921 0.639 !       0.74 eA-3
Q146 0.209 0.401 0.231 !       0.74 eA-3
Q147 0.187 0.313 0.748 !       0.74 eA-3
Q148 0.841 0.708 0.232 !       0.74 eA-3
Q149 0.467 0.278 0.881 !       0.73 eA-3
Q150 0.516 0.097 0.037 !       0.73 eA-3
Q151 0.299 0.974 0.764 !       0.73 eA-3
C152 0.906 0.136 0.435 !       0.73 eA-3
C153 0.083 0.783 0.980 !       0.73 eA-3
C154 0.949 0.182 0.514 !       0.73 eA-3
Q155 0.688 0.653 0.868 !       0.72 eA-3
Q156 0.531 0.685 0.144 !       0.72 eA-3
Q157 0.076 0.301 0.665 !       0.72 eA-3
C158 0.125 0.945 0.397 !       0.72 eA-3
Q159 0.064 0.309 0.790 !       0.71 eA-3
Q160 0.469 0.702 0.163 !       0.71 eA-3
Q161 0.579 0.126 0.528 !       0.71 eA-3
Q162 0.766 0.722 0.232 !       0.70 eA-3
Q163 0.159 0.109 0.968 !       0.70 eA-3
C164 0.812 0.952 0.699 !       0.70 eA-3
Q165 0.364 0.205 0.282 !       0.70 eA-3
Q166 0.220 0.635 0.924 !       0.69 eA-3
Q167 0.362 0.203 0.308 !       0.69 eA-3
Q168 0.597 0.310 0.203 !       0.69 eA-3
Q169 0.265 0.248 0.395 !       0.69 eA-3
Q170 0.859 0.731 0.483 !       0.69 eA-3
C171 0.845 0.394 0.129 !       0.68 eA-3
Q172 0.095 0.926 0.952 !       0.68 eA-3
Q173 0.376 0.343 0.201 !       0.68 eA-3
Q174 0.432 0.563 0.607 !       0.68 eA-3
Q175 0.080 1.002 0.030 !       0.68 eA-3
C176 0.968 0.661 0.986 !       0.68 eA-3
Q177 0.530 0.685 0.339 !       0.68 eA-3
Q178 0.982 0.690 0.139 !       0.68 eA-3
Q179 0.470 0.812 0.174 !       0.68 eA-3
Q180 0.630 0.243 0.932 !       0.68 eA-3
Q181 0.575 0.598 0.957 !       0.67 eA-3
Q182 0.448 0.733 0.375 !       0.67 eA-3
Q183 0.048 0.831 0.261 !       0.67 eA-3
Q184 0.912 0.078 0.720 !       0.67 eA-3
Q185 0.482 0.815 0.338 !       0.67 eA-3
Q186 0.064 0.434 0.498 !       0.67 eA-3
Q187 0.360 0.855 0.642 !       0.67 eA-3
Q188 0.922 0.367 0.747 !       0.67 eA-3
Q189 0.234 0.750 0.644 !       0.67 eA-3
Q190 0.454 0.371 0.071 !       0.66 eA-3
Q191 0.331 0.258 0.935 !       0.66 eA-3
Q192 0.641 0.230 0.786 !       0.66 eA-3
Q193 0.485 0.202 0.655 !       0.65 eA-3
Q194 0.267 0.862 0.860 !       0.65 eA-3
Q195 0.721 0.957 0.654 !       0.65 eA-3
C196 0.952 0.999 0.675 !       0.65 eA-3
Q197 0.499 0.614 0.439 !       0.65 eA-3
Q198 0.438 0.241 0.877 !       0.65 eA-3
C199 0.120 0.079 0.367 !       0.65 eA-3
(replace by semicolon in column 1 when used as .sqf)
;
_refine_diff_density_max         3.204
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         22056
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2967
_refine_ls_wR_factor_ref         0.3199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15092
_reflns_number_total             22056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00480b2.cif
_cod_data_source_block           exp_6
_cod_depositor_comments
'Adding full bibliography for 7034568--7034573.cif.'
_cod_original_formula_sum        'C78 H88 Br6 Ca2.50 N12 O20'
_cod_database_code               7034573
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H7A-H28D
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: O28(0.5) H28C(0.5) H28D(0.5) O1A(0.5) H1AA(0.5) H1AB(0.5) Ca1B(0.5)
4.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10C,H10D), O11(H11A,H11B),
 O12(H12A,H12B), O13(H13A,H13B), O28(H28C,H28D), O1A(H1AA,H1AB)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C20(H20A,H20B), C28(H28A,H28B), C30(H30A,H30B),
 C38(H38A,H38B), C41(H41A,H41B), C49(H49A,H49B), C59(H59A,H59B), C67(H67A,H67B),
  C69(H69A,H69B), C77(H77A,H77B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C22(H22), C23(H23), C24(H24),
 C25(H25), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C61(H61), C62(H62), C63(H63),
 C64(H64), C66(H66), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_shelx_fab_checksum              43199
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'