Solvent-regulated biomorphs from the intense π,π-mediated assemblies of tetracenequinone fused porphyrin
Chen, Chen; Li, Dan; Cao, Guanyue; Qin, Zhonghe; Xu, Yi; Liu, Xiujun; Li, Qizhao; Xie, Yongshu; Li, Chengjie; CrystEngComm 23 (2021) 7565–7569; doi:10.1039/D1CE01173A

data_7243657
_publ_section_title
;
 Solvent-regulated biomorphs from the intense \p,\p-mediated assemblies of
 tetracenequinone fused porphyrin
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7565
_journal_page_last               7569
_journal_paper_doi               10.1039/D1CE01173A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C124 H108 N4 Ni O8'
_chemical_formula_sum            'C124 H108 N4 Ni O8'
_chemical_formula_weight         1840.85
_chemical_melting_point_gt       573
_chemical_name_systematic        Ni4AQ
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-10 deposited with the CCDC.	2021-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.271(2)
_cell_length_b                   22.271(2)
_cell_length_c                   12.5290(16)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      67.89
_cell_measurement_theta_min      4.51
_cell_volume                     6214.4(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295.0
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.817
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.817
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            48412
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.520
_diffrn_reflns_theta_min         3.970
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1642 before and 0.0950 after correction.
The Ratio of minimum to maximum transmission is 0.7834.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.31
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5273
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0972
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2893
_refine_ls_wR_factor_ref         0.3111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3657
_reflns_number_total             5273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01173a2.cif
_cod_data_source_block           cc4022_0ma_c
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_melting_point_gt' since the value was specified as 'more
than' ('>') a certain temperature. The value '>573 K' was changed to
'573' -- it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7243657--7243658.cif.
;
_cod_original_cell_volume        6214.2(15)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7243657
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 C2, C2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N002 \\sim C005 \\sim C008 \\sim C00C \\sim C00G \\sim C00F \\sim C00E \\sim
C006 \\sim C00A \\sim C007 \\sim C009 \\sim C22 \\sim C00K \\sim C00O \\sim
C00N \\sim C00B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C00K \\sim C00O \\sim C00N \\sim C00B \\sim C009 \\sim C22: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C00N \\sim C00B \\sim C009 \\sim C22 \\sim C00K \\sim C00O: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C7) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C9) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C6A) \\sim Ueq, Uanis(C6B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) = Uanis(C2A)
4. Rigid body (RIGU) restrains
 N002, C00A, C008, C009, C00B, C005, C006, C007, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=1-FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=FVAR(1)
 Fixed Sof: C2(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) H3BD(0.5) H3BE(0.5)
 H3BF(0.5) C2A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00E(H00E), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C21(H21), C22(H22)
6.b Idealised Me refined as rotating group:
 C3(H3AA,H3AB,H3AC), C3(H3BD,H3BE,H3BF), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,H6BC), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37728
_shelx_hkl_checksum              77963
_shelx_fab_checksum              91497
_olex2_submission_special_instructions 'No special instructions were received'