Modulating the structure and photochromic performance of hybrid metal chloride with nonphotochromic 1,10-phenanthroline and its derivative
Xu, Fei; Li, Gang-Mei; Wang, Ani; Han, Song-De; Pan, Jie; Wang, Guo-Ming; Dalton Transactions  (2021) –; doi:10.1039/D1DT02899E

data_7708796
_publ_section_title
;
 Modulating the structure and photochromic performance of hybrid metal
 chloride with nonphotochromic 1,10-phenanthroline and its derivative
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02899E
_journal_year                    2021
_chemical_formula_moiety         'C24 H14 Cl6 N4 Pb2'
_chemical_formula_sum            'C24 H14 Cl6 N4 Pb2'
_chemical_formula_weight         985.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-09-15
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.692(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9182(9)
_cell_length_b                   10.8666(5)
_cell_length_c                   8.1504(6)
_cell_measurement_reflns_used    2533
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1460
_cell_measurement_theta_min      2.6750
_cell_volume                     1343.15(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3738
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         2.306
_exptl_absorpt_coefficient_mu    13.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;     

CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,

implemented in SCALE3 ABSPACK scaling algorithm.

;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_description       stick
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.999
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1182
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0610P)^2^+14.4644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1058
_reflns_number_total             1182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02899e2.cif
_cod_data_source_block           6
_cod_database_code               7708796
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5_$1-C5A = C5A-C4A = C4A-C6A = C6A-C6_$1 = C6_$1-C4_$1 = C4_$1-C5_$1
 1.39 with sigma of 0.01
 C5-C5A_$1 = C5A_$1-C4A_$1 = C4A_$1-C6A_$1 = C6A_$1-C6 = C6-C4 = C4-C5
 1.39 with sigma of 0.01
 Pb1-N1 \\sim Pb1-N1A
 with sigma of 0.02
 C5_$1-C4A \\sim C5A-C6A \\sim C4A-C6_$1 \\sim C6A-C4_$1 \\sim C6_$1-C5_$1
\\sim C4_$1-C5A
 with sigma of 0.02
 C5-C4A_$1 \\sim C5A_$1-C6A_$1 \\sim C4A_$1-C6 \\sim C6A_$1-C4 \\sim C6-C5
\\sim C4-C5A_$1
 with sigma of 0.02
3. Restrained planarity
 C5_$1, C5A, C4A, C6A, C6_$1, C4_$1
 with sigma of 0.1
 C5, C5A_$1, C4A_$1, C6A_$1, C6, C4
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1A \\sim N1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(Cl1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N1(0.5) C3(0.5) H3(0.5) C1(0.5) H1(0.5) C4(0.5) Cl1(0.32) C6(0.5)
 H6(0.5) C5(0.5) C2(0.5) H2(0.5) Cl2B(0.5) N1A(0.5) C3A(0.5) H3A(0.5) C1A(0.5)
 H1A(0.5) C4A(0.5) Cl1A(0.18) C6A(0.5) H6A(0.5) C5A(0.5) C2A(0.5) H2A(0.5)
 Cl2A(0.5)
7.a Riding coordinates:
 C6(H6), C6A(H6A)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), C2(H2), C3A(H3A), C1A(H1A), C2A(H2A)
;
_shelx_res_checksum              39900
_olex2_submission_special_instructions 'No special instructions were received'