Calcium-based efficient cathode-ray scintillating metal-organic frameworks constructed from π-conjugated luminescent motifs
Lu, Jian; Wu, Hui-Fang; Wang, Wen-Fei; Xu, Jian-Gang; Zheng, Fa-Kun; Guo, Guo-Cong; Chemical Communications  (2019) –; doi:10.1039/C9CC06760D

data_7124363
_publ_section_title
;
 Calcium-based efficient cathode-ray scintillating metal-organic
 frameworks constructed from \p-conjugated luminescent motifs
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06760D
_journal_year                    2019
_chemical_formula_moiety         'C56 H44 Ca2 N4 O10, 0.5(H2 O)'
_chemical_formula_sum            'C56 H45 Ca2 N4 O10.5'
_chemical_formula_weight         1022.12
_chemical_melting_point          ?
_chemical_name_common            '[Ca2(L2)2(DMF)2]n,0.5nH2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-26 deposited with the CCDC.    2019-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.879(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9576(3)
_cell_length_b                   13.2038(3)
_cell_length_c                   37.1629(13)
_cell_measurement_reflns_used    12335
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6960
_cell_measurement_theta_min      1.8950
_cell_volume                     4879.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.797
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            43938
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.086
_diffrn_reflns_theta_min         1.893
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       sheet
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12492
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0394P)^2^+8.3255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9016
_reflns_number_total             12492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06760d2.cif
_cod_data_source_block           Ca-SMOF-2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C56 H45 Ca2 N4 O10.50'
_cod_database_code               7124363
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O10-C54 = O10-C54B
 1.25 with sigma of 0.01
 N4-C54 = N4-C55 = N4-C56 = N4B-C54B = N4B-C55B = N4B-C56B
 1.42 with sigma of 0.02
 C54-C55 \\sim C54-C56 \\sim C54B-C55B \\sim C54B-C56B \\sim C55-C56 \\sim
C55B-C56B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N4 \\sim C54 \\sim C55 \\sim C56 \\sim N4B \\sim C54B \\sim C55B \\sim C56B:
within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(N4B)=Sof(C54B)=Sof(H54B)=Sof(C55B)=Sof(H55D)=Sof(H55E)=Sof(H55F)=
 Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(N4)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=
 Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
5.a Riding coordinates:
 N2(H2)
5.b Free rotating group:
 O1W(H1WA,H1WB)
5.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C34(H34A,H34B)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C6(H6), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C28(H28), C31(H31), C33(H33),
  C36(H36), C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
 C46(H46), C47(H47), C51(H51), C54(H54), C54B(H54B)
5.e Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C55B(H55D,H55E,H55F), C56B(H56D,H56E,H56F)
;
_shelx_res_checksum              43689
_olex2_submission_special_instructions 'No special instructions were received'