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_7124362
_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         'C52 H42.72 Ca2 N4 O11'
_chemical_formula_sum            'C52 H46 Ca2 N4 O11'
_chemical_formula_weight         983.09
_chemical_melting_point          ?
_chemical_name_common            '[Ca2(L1)2(DMF)2(H2O)]n'
_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     dual
_audit_creation_date             2019-07-18
_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                94.7350(10)
_cell_angle_beta                 96.2260(10)
_cell_angle_gamma                103.502(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9541(2)
_cell_length_b                   15.0085(3)
_cell_length_c                   16.4447(3)
_cell_measurement_reflns_used    45607
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2800
_cell_measurement_theta_min      3.9180
_cell_volume                     2359.95(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23b (Rigaku OD, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.931
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            191912
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.454
_diffrn_reflns_theta_min         3.763
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         14571
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+1.1782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12599
_reflns_number_total             14571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06760d2.cif
_cod_data_source_block           Ca-SMOF-1
_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_database_code               7124362
_shelx_shelxl_version_number     2017/1
_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
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 N2-H2 = N1-H1
 0.89 with sigma of 0.02
 C50-O10 = C50B-O10B
 1.25 with sigma of 0.02
 C47-O9 = C47-O9 = C47B-O9
 1.25 with sigma of 0.02
 C47-N3 = N3-C47B
 1.4 with sigma of 0.02
 C50-C51 = C50-C52 = C50B-C51B = C50B-C52B
 2.35 with sigma of 0.02
 C47-C48 = C47-C49 = C47B-C48B = C47B-C49B
 2.35 with sigma of 0.02
 C51-C52 = C51B-C52B = C48B-C49B = C48-C49
 2.4 with sigma of 0.02
 N4-C51 = N4-C52 = N4B-C51B = N4B-C52B
 1.42 with sigma of 0.02
 N3-C48 = N3-C49 = N3-C48B = N3-C49B
 1.42 with sigma of 0.02
 H1WA-H1WB
 1.39 with sigma of 0.01
 O10-N4 \\sim O10B-N4B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C47 \\sim C48 \\sim C49 \\sim C47B \\sim C48B \\sim C49B: within 3.8A with
sigma of 0.03 and sigma for terminal atoms of 0.06
O10 \\sim N4 \\sim C50 \\sim C51 \\sim C52 \\sim O10B \\sim N4B \\sim C50B
\\sim C51B \\sim C52B: within 3.8A with sigma of 0.03 and sigma for terminal
atoms of 0.06
Uanis(C52) \\sim Ueq, Uanis(C49B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49B)=
 Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(O10B)=Sof(N4B)=Sof(C50B)=Sof(H50B)=Sof(C51B)=
 Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52B)=Sof(H52A)=Sof(H52B)=Sof(H52C)=1-FVAR(1)
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=
 Sof(H49B)=Sof(H49C)=Sof(O10)=Sof(N4)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(C52)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C32(H32A,H32B)
5.b Me refined with riding coordinates:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C48B(H48D,H48E,H48F), C49B(H49D,
 H49E,H49F), C51B(H51A,H51B,H51C), C52B(H52A,H52B,H52C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22), C26(H26), C29(H29), C31(H31), C35(H35),
  C36(H36), C37(H37), C38(H38), C40(H40), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C47B(H47B), C50(H50), C50B(H50B)
;
_shelx_res_checksum              11051
_olex2_submission_special_instructions 'No special instructions were received'