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_7034572
_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
'C54 H66.5 Br0.15 Ca2.5 Cl0.85 N12 Na O17.25, 3(H2 O), 5.5(Br), 1.5(O)'
_chemical_formula_sum            'C54 H72.5 Br5.65 Ca2.5 Cl0.85 N12 Na O21.75'
_chemical_formula_weight         1842.55
_chemical_name_systematic        5
_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
_audit_creation_date             2015-02-07
_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                103.011(4)
_cell_angle_beta                 107.177(5)
_cell_angle_gamma                99.571(4)
_cell_formula_units_Z            2
_cell_length_a                   14.4574(8)
_cell_length_b                   15.3803(6)
_cell_length_c                   19.4570(11)
_cell_measurement_reflns_used    13766
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.01
_cell_measurement_theta_min      3.30
_cell_volume                     3899.4(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 0.929
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27821
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.700
_diffrn_reflns_theta_max         71.006
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.896
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.170
_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    1.569
_exptl_crystal_description       Block
_exptl_crystal_F_000             1855
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00046(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         13719
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0837
_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^)+(0.1600P)^2^+3.2301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10621
_reflns_number_total             13719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00480b2.cif
_cod_data_source_block           exp_5
_cod_depositor_comments
'Adding full bibliography for 7034568--7034573.cif.'
_cod_original_formula_sum
'C54 H72.50 Br5.65 Ca2.50 Cl0.85 N12 Na O21.75'
_cod_database_code               7034572
_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
 C3A-C4B
 2.3 with sigma of 0.02
 H15A-H14B
 2.2 with sigma of 0.02
 H9A-H40A
 2.2 with sigma of 0.02
3. Restrained planarity
 C3B, C4B, N3, N4
 with sigma of 0.1
 C3B, C4B, N3, N4
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O9: within 1.2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C3B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: Br5(0.15) C3A(0.5) H3AA(0.5) C3B(0.5) H3BA(0.5) C4A(0.5) H4A(0.5)
 C4B(0.5) H4B(0.5) Ca4(0.5) Cl1(0.85) O1B(0.5) O1C(0.25) H1CA(0.25) H1CB(0.25)
 O4(0.5) H4C(0.5) H4D(0.5) O8(0.5) O12(0.5) H12A(0.5) H12B(0.5) O16A(0.5)
 O16B(0.5) Br2A(0.16) Br2B(0.34) Br4B(0.2) Br4C(0.15) Br1B(0.5) Br4A(0.65)
 Br8(0.1) O2A(0.5) Br1A(0.5) O1E(0.5) O2B(0.5) Br7(0.9)
6.a Free rotating group:
 O9(H9A,H9B), O24(H24A,H24B), O15(H15C,H15D)
6.b Rotating group:
 O1C(H1CA,H1CB), O4(H4C,H4D), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B)
6.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C15(H15A,H15B), C16(H16A,H16B), C20(H20A,H20B),
 C26(H26A,H26B), C29(H29A,H29B), C33(H33A,H33B), C43(H43A,H43B), C47(H47A,H47B),
  C49(H49A,H49B), C53(H53A,H53B)
6.d Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C3A(H3AA), C3AA(H3AB), C3B(H3BA), C4A(H4A), C4AA(H4AA), C4B(H4B),
 C17(H17), C18(H18), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C44(H44),
  C45(H45), C46(H46), C50(H50), C51(H51), C52(H52)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              38117
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'