Supramolecular frameworks based on 5,10,15,20-tetra(4-carboxyphenyl)porphyrins.
Morshedi, Mahbod; Ward, Jas S.; Kruger, Paul E.; White, Nicholas G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 783–790; doi:10.1039/c7dt04162d

data_7045055
_publ_section_title
;
 Supramolecular frameworks based on
 5,10,15,20-tetra(4-carboxyphenyl)porphyrins.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              783
_journal_page_last               790
_journal_paper_doi               10.1039/c7dt04162d
_journal_volume                  47
_journal_year                    2018
_chemical_compound_source        synthesized
_chemical_formula_moiety         '1.5(C48 H26 N4 O8), 3(C8 H12 N4)'
_chemical_formula_sum            'C96 H75 N18 O12'
_chemical_formula_weight         1672.76
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                86.1854(13)
_cell_angle_beta                 79.7696(15)
_cell_angle_gamma                72.5303(15)
_cell_formula_units_Z            2
_cell_length_a                   15.6606(3)
_cell_length_b                   18.9312(3)
_cell_length_c                   20.4250(3)
_cell_measurement_reflns_used    25303
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.7
_cell_measurement_theta_min      2.20
_cell_volume                     5683.78(17)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            118047
_diffrn_reflns_theta_full        72.698
_diffrn_reflns_theta_max         74.181
_diffrn_reflns_theta_min         2.447
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1746
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         2.72
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1216
_refine_ls_number_reflns         22854
_refine_ls_number_restraints     287
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.0003973
_refine_ls_shift/su_mean         0.0000410
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 908. 0.151E+04 888. 349. 73.2 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2250
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2245
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                18002
_reflns_number_total             22953
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.44
_oxford_diffrn_Wilson_scale      0.63
_oxford_refine_ls_r_factor_ref   0.0929
_oxford_refine_ls_scale          1.380(5)
_oxford_reflns_number_all        22859
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt04162d2.cif
_cod_data_source_block           2_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7045051--7045058.cif.
;
_cod_original_cell_volume        5683.78(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7045055
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT N    (  101 ,X'S,U'S)  UNTIL C    (   69 ) 
CONT H    ( 2251 ,X'S)  UNTIL H    ( 2052 ) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) 
RIDE C   ( 146,X'S) H   (1461,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) 
RIDE C   ( 149,X'S) H   (1491,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 228,X'S) H   (2281,X'S) 
RIDE C   ( 229,X'S) H   (2291,X'S) 
RIDE C   ( 231,X'S) H   (2311,X'S) 
RIDE C   ( 232,X'S) H   (2321,X'S) 
RIDE C   ( 245,X'S) H   (2451,X'S) 
RIDE C   ( 246,X'S) H   (2461,X'S) 
RIDE C   ( 265,X'S) H   (2651,X'S) 
RIDE C   ( 266,X'S) H   (2661,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
END      
;
_iucr_refine_instructions_details_restraints
;                                                                       
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM            H1-N-R2 
DIST 0.86, 0.02 = 
CONT N ( 107) TO H(1071) 
REST 0.028, 0.002 = H(1071,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(1071) TO N ( 107) TO C(108) 
CONT H(1071) TO N ( 107) TO C(111) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 201) TO H(2011) 
CONT N ( 201) TO H(2012) 
REST 0.081, 0.002 = H(2011,U[ISO]) 
REST 0.081, 0.002 = H(2012,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(203) TO N ( 201) TO H(2011) 
CONT C(203) TO N ( 201) TO H(2012) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 202) TO H(2021) 
CONT N ( 202) TO H(2022) 
REST 0.071, 0.002 = H(2021,U[ISO]) 
REST 0.071, 0.002 = H(2022,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(203) TO N ( 202) TO H(2021) 
CONT C(203) TO N ( 202) TO H(2022) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 204) TO H(2041) 
CONT N ( 204) TO H(2042) 
REST 0.068, 0.002 = H(2041,U[ISO]) 
REST 0.068, 0.002 = H(2042,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(206) TO N ( 204) TO H(2041) 
CONT C(206) TO N ( 204) TO H(2042) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 205) TO H(2051) 
CONT N ( 205) TO H(2052) 
REST 0.072, 0.002 = H(2051,U[ISO]) 
REST 0.072, 0.002 = H(2052,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(206) TO N ( 205) TO H(2051) 
CONT C(206) TO N ( 205) TO H(2052) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 221) TO H(2212) 
CONT N ( 221) TO H(2211) 
REST 0.032, 0.002 = H(2212,U[ISO]) 
REST 0.032, 0.002 = H(2211,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(223) TO N ( 221) TO H(2212) 
CONT C(223) TO N ( 221) TO H(2211) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 222) TO H(2221) 
CONT N ( 222) TO H(2222) 
REST 0.038, 0.002 = H(2221,U[ISO]) 
REST 0.038, 0.002 = H(2222,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(223) TO N ( 222) TO H(2221) 
CONT C(223) TO N ( 222) TO H(2222) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 224) TO H(2241) 
CONT N ( 224) TO H(2242) 
REST 0.031, 0.002 = H(2241,U[ISO]) 
REST 0.031, 0.002 = H(2242,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(226) TO N ( 224) TO H(2241) 
CONT C(226) TO N ( 224) TO H(2242) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 225) TO H(2251) 
CONT N ( 225) TO H(2252) 
REST 0.033, 0.002 = H(2251,U[ISO]) 
REST 0.033, 0.002 = H(2252,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(226) TO N ( 225) TO H(2251) 
CONT C(226) TO N ( 225) TO H(2252) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 241) TO H(2412) 
CONT N ( 241) TO H(2411) 
REST 0.031, 0.002 = H(2412,U[ISO]) 
REST 0.031, 0.002 = H(2411,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(243) TO N ( 241) TO H(2412) 
CONT C(243) TO N ( 241) TO H(2411) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 242) TO H(2422) 
CONT N ( 242) TO H(2421) 
REST 0.034, 0.002 = H(2422,U[ISO]) 
REST 0.034, 0.002 = H(2421,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(243) TO N ( 242) TO H(2422) 
CONT C(243) TO N ( 242) TO H(2421) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 261) TO H(2611) 
CONT N ( 261) TO H(2612) 
REST 0.122, 0.002 = H(2611,U[ISO]) 
REST 0.122, 0.002 = H(2612,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(263) TO N ( 261) TO H(2611) 
CONT C(263) TO N ( 261) TO H(2612) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 262) TO H(2621) 
CONT N ( 262) TO H(2622) 
REST 0.138, 0.002 = H(2621,U[ISO]) 
REST 0.138, 0.002 = H(2622,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(263) TO N ( 262) TO H(2621) 
CONT C(263) TO N ( 262) TO H(2622) 
REM            H1-N-R2 
DIST 0.86, 0.02 = 
CONT N ( 7) TO H(71) 
REST 0.025, 0.002 = H(71,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(71) TO N ( 7) TO C(8) 
CONT H(71) TO N ( 7) TO C(11) 
REM            H1-N-R2 
DIST 0.86, 0.02 = 
CONT N ( 19) TO H(191) 
REST 0.026, 0.002 = H(191,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(191) TO N ( 19) TO C(20) 
CONT H(191) TO N ( 19) TO C(23) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM 
REM POORLY-BEHAVED BENZOATES 
REM 
DIST 1.40, 0.005= C(54) TO C(55), C(55) TO C(56) 
CONT C(56) TO C(57), C(57) TO C(58) 
CONT C(58) TO C(59), C(59) TO C(54) 
CONT C(144) TO C(145), C(145) TO C(146) 
CONT C(146) TO C(147), C(147) TO C(148) 
CONT C(148) TO C(149), C(149) TO C(144) 
DIST 1.49, 0.005 = C(53) TO C(54), C(143) TO C(144) 
DIST 1.25, 0.005 = O(51) TO C(53), O(52) TO C(53) 
CONT O(141) TO C(143), O(142) TO C(143) 
REM POORLY-BEHAVED AMIDINIUM 
DIST 1.31, 0.005 = N(261) TO C(263), N(262) TO C(263) 
DIST 1.49, 0.005 = C(263) TO C(264) 
DIST 1.40, 0.005 = C(264) TO C(265), C(264) TO C(266) 
CONT C(265) TO C(266,-1,1,0,2), C(266) TO C(265,-1,1,0,2) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00100 = O(141) TO C(143) 
VIBR .0, 0.00100 = O(142) TO C(143) 
VIBR .0, 0.00100 = C(143) TO C(144) 
VIBR .0, 0.00200 = O(141) TO O(142) 
VIBR .0, 0.00200 = C(144) TO O(142) 
VIBR .0, 0.00200 = C(144) TO O(141) 
VIBR .0, 0.00100 = C(144) TO C(145) 
VIBR .0, 0.00100 = C(144) TO C(149) 
VIBR .0, 0.00200 = C(145) TO C(143) 
VIBR .0, 0.00200 = C(149) TO C(143) 
VIBR .0, 0.00200 = C(149) TO C(145) 
VIBR .0, 0.00100 = C(145) TO C(146) 
VIBR .0, 0.00200 = C(146) TO C(144) 
VIBR .0, 0.00100 = C(146) TO C(147) 
VIBR .0, 0.00200 = C(147) TO C(145) 
VIBR .0, 0.00100 = C(147) TO C(148) 
VIBR .0, 0.00200 = C(146) TO C(112) 
VIBR .0, 0.00200 = C(148) TO C(112) 
VIBR .0, 0.00200 = C(148) TO C(146) 
VIBR .0, 0.00100 = C(148) TO C(149) 
VIBR .0, 0.00200 = C(149) TO C(147) 
VIBR .0, 0.00200 = C(148) TO C(144) 
VIBR .0, 0.00100 = N(261) TO C(263) 
VIBR .0, 0.00100 = N(262) TO C(263) 
VIBR .0, 0.00100 = C(263) TO C(264) 
VIBR .0, 0.00200 = N(261) TO N(262) 
VIBR .0, 0.00200 = C(264) TO N(262) 
VIBR .0, 0.00200 = C(264) TO N(261) 
VIBR .0, 0.00100 = C(264) TO C(265) 
VIBR .0, 0.00100 = C(264) TO C(266) 
VIBR .0, 0.00200 = C(265) TO C(263) 
VIBR .0, 0.00200 = C(266) TO C(263) 
VIBR .0, 0.00200 = C(266) TO C(265) 
VIBR .0, 0.00100 = C(265) TO C(266,-1,1,0,2) 
VIBR .0, 0.00200 = C(266,-1,1,0,2) TO C(264) 
VIBR .0, 0.00200 = C(264) TO C(265,-1,1,0,2) 
VIBR .0, 0.00100 = C(48) TO C(49) 
VIBR .0, 0.00200 = C(49) TO C(47) 
VIBR .0, 0.00200 = C(44) TO C(48) 
VIBR .0, 0.00100 = O(51) TO C(53) 
VIBR .0, 0.00100 = O(52) TO C(53) 
VIBR .0, 0.00100 = C(53) TO C(54) 
VIBR .0, 0.00200 = O(51) TO O(52) 
VIBR .0, 0.00200 = C(54) TO O(52) 
VIBR .0, 0.00200 = C(54) TO O(51) 
VIBR .0, 0.00100 = C(54) TO C(55) 
VIBR .0, 0.00100 = C(54) TO C(59) 
VIBR .0, 0.00200 = C(55) TO C(53) 
VIBR .0, 0.00200 = C(59) TO C(53) 
VIBR .0, 0.00200 = C(59) TO C(55) 
VIBR .0, 0.00100 = C(55) TO C(56) 
VIBR .0, 0.00200 = C(56) TO C(54) 
VIBR .0, 0.00100 = C(56) TO C(57) 
VIBR .0, 0.00200 = C(57) TO C(55) 
VIBR .0, 0.00100 = C(57) TO C(58) 
VIBR .0, 0.00200 = C(56) TO C(12) 
VIBR .0, 0.00200 = C(58) TO C(12) 
VIBR .0, 0.00200 = C(58) TO C(56) 
VIBR .0, 0.00100 = C(58) TO C(59) 
VIBR .0, 0.00200 = C(59) TO C(57) 
VIBR .0, 0.00200 = C(54) TO C(58) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.02000 = O(141) TO C(143) 
U(IJ) .0, 0.02000 = O(142) TO C(143) 
U(IJ) .0, 0.01000 = C(143) TO C(144) 
U(IJ) .0, 0.01000 = C(144) TO C(145) 
U(IJ) .0, 0.01000 = C(144) TO C(149) 
U(IJ) .0, 0.01000 = C(145) TO C(146) 
U(IJ) .0, 0.01000 = C(146) TO C(147) 
U(IJ) .0, 0.01000 = C(147) TO C(148) 
U(IJ) .0, 0.01000 = C(148) TO C(149) 
U(IJ) .0, 0.02000 = N(261) TO C(263) 
U(IJ) .0, 0.02000 = N(262) TO C(263) 
U(IJ) .0, 0.01000 = C(263) TO C(264) 
U(IJ) .0, 0.01000 = C(264) TO C(265) 
U(IJ) .0, 0.01000 = C(264) TO C(266) 
U(IJ) .0, 0.01000 = C(265) TO C(266,-1,1,0,2) 
U(IJ) .0, 0.02000 = O(51) TO C(53) 
U(IJ) .0, 0.02000 = O(52) TO C(53) 
U(IJ) .0, 0.01000 = C(53) TO C(54) 
U(IJ) .0, 0.01000 = C(54) TO C(55) 
U(IJ) .0, 0.01000 = C(54) TO C(59) 
U(IJ) .0, 0.01000 = C(55) TO C(56) 
U(IJ) .0, 0.01000 = C(56) TO C(57) 
U(IJ) .0, 0.01000 = C(57) TO C(58) 
U(IJ) .0, 0.01000 = C(58) TO C(59) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;