The impact of metal cations on photochemical properties of hybrid heterostructures with infinite alkaline-earth metal oxide clusters
You, Ming-Hua; Li, Meng-Hua; Li, Hao-Hong; Chen, Yong; Lin, Mei-Jin; Dalton Transactions  (2019) –; doi:10.1039/C9DT04104D

data_7701491
_publ_section_title
;
 The impact of metal cations on photochemical properties of hybrid
 heterostructures with infinite alkaline-earth metal oxide clusters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04104D
_journal_year                    2019
_chemical_formula_moiety         'C21 H19 Ca N3 O8, 1[C3H7NO]'
_chemical_formula_sum            'C24 H26 Ca N4 O9'
_chemical_formula_weight         554.57
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc22k8zx
_audit_creation_date             2019-10-28
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.10.03 svn.r3666 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2019-10-29 deposited with the CCDC.	2019-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.1585(17)
_cell_length_b                   28.1585(17)
_cell_length_c                   13.4560(16)
_cell_measurement_reflns_used    2366
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.3160
_cell_measurement_theta_min      3.7510
_cell_volume                     10669.3(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -79.00 -53.00   0.50   45.00    --   -9.60  31.00  22.00   52
  2  \w    -98.00 -73.00   0.50   45.00    --   -9.60  55.00-150.00   50
  3  \w    -43.00  78.00   0.50   45.00    --   -9.60  55.00-150.00  242
  4  \w    -23.00   2.00   0.50   45.00    --   -9.60  31.00  22.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23227
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.655
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0829P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2563
_reflns_number_total             4698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04104d2.cif
_cod_data_source_block           ca_1020
_cod_original_cell_volume        10669.3(18)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7701491
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8195(18)
 0.1805(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C11(H11), C19(H19), C18(H18), C5(H5), C3(H3)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78525
_shelx_fab_checksum              26375
_platon_squeeze_special_details
;
A solvent mask was calculated and 540 electrons were
found in a volume of 2452\%A^3 in 1 void per unit cell.
This is reasonably consistent with the presence of 1[C3H7NO]
per Formula Unit which account for 640 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;