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_7034569
_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
'Br O2, 2(Br), Br O1.77, C58 H72.4 Ca2 N8 O16.2, 4(H2 O)'
_chemical_formula_sum            'C58 H80.4 Br4 Ca2 N8 O23.97'
_chemical_formula_weight         1673.02
_chemical_name_systematic        2
_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             2015-02-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                94.247(4)
_cell_angle_beta                 109.921(4)
_cell_angle_gamma                110.838(5)
_cell_formula_units_Z            2
_cell_length_a                   14.1675(7)
_cell_length_b                   16.5118(9)
_cell_length_c                   17.3328(8)
_cell_measurement_reflns_used    13074
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.85
_cell_measurement_theta_min      3.57
_cell_volume                     3473.6(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26432
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.853
_diffrn_reflns_theta_min         3.569
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       Block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.649
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.139
_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     886
_refine_ls_number_reflns         13074
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1269P)^2^+6.8602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10119
_reflns_number_total             13074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00480b2.cif
_cod_data_source_block           exp_2
_cod_depositor_comments
'Adding full bibliography for 7034568--7034573.cif.'
_cod_original_cell_volume        3473.6(3)
_cod_original_formula_sum        'C58 H80.40 Br4 Ca2 N8 O23.97'
_cod_database_code               7034569
_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
 H7D-H3AA
 2.2 with sigma of 0.02
 H7C-H3AA
 2.2 with sigma of 0.02
 H3AB-H2AB
 2.2 with sigma of 0.02
 H17A-H29A
 2.3 with sigma of 0.02
 H10A-H27A
 2.3 with sigma of 0.02
 H25A-H2BA
 2.2 with sigma of 0.02
 H7D-H4BA
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: O3A(0.7) H3AA(0.7) H3AB(0.7) O4A(0.6) H4AA(0.6) H4AB(0.6)
 O6A(0.85) O7(0.5) H7C(0.5) H7D(0.5) O1(0.77) O6B(0.15) O4B(0.4) H4BA(0.4)
 H4BB(0.4)
4.a Free rotating group:
 C19A(C20A,C21A,O2B), C22A(C23A,C24A,C25A,C26A,C27A,C28A,C29A,Ca2,O1B), O9(H9A,
 H9B), O(HA,HB), O2(H2A,H2B,O3)
4.b Rotating group:
 O1A(H1A,H1AA), O2A(H2AA,H2AB), O3A(H3AA,H3AB), O4A(H4AA,H4AB), O2B(H2BA,H2BB),
  O1B(H1BA,H1BB), O9A(H9AA,H9AB), O14(H14A,H14B), O7(H7C,H7D), O4B(H4BA,H4BB)
4.c Secondary CH2 refined with riding coordinates:
 C2A(H2AC,H2AD), C10A(H10A,H10B), C17A(H17A,H17B), C25A(H25A,H25B), C2B(H2BC,
 H2BD), C10B(H10C,H10D), C17B(H17C,H17D), C25B(H25C,H25D)
4.d Me refined with riding coordinates:
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C27B(H27D,
 H27E,H27F), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F)
4.e Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C13A(H13A), C18A(H18A),
 C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C3B(H3B), C5B(H5B), C6B(H6B),
 C7B(H7B), C8B(H8B), C13B(H13B), C18B(H18B), C20B(H20B), C21B(H21B), C22B(H22B),
  C23B(H23B)
;
_shelx_res_checksum              32684
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'