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_7045054
_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
'C48 H26 N4 O8, 2(C8 H12 N4), 3(C5 H5 N), H2 O'
_chemical_formula_sum            'C79 H67 N15 O9'
_chemical_formula_weight         1370.50
_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                109.178(2)
_cell_angle_beta                 103.485(2)
_cell_angle_gamma                103.585(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0854(2)
_cell_length_b                   20.0861(5)
_cell_length_c                   20.4927(5)
_cell_measurement_reflns_used    15751
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.7
_cell_measurement_theta_min      2.20
_cell_volume                     3586.88(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.029
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            118047
_diffrn_reflns_theta_full        68.240
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         2.476
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_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    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9755
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         13004
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.0003970
_refine_ls_shift/su_mean         0.0000260
_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: 
 961. 0.152E+04 880. 328. 60.4 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1204
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1202
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              -24
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10787
_reflns_number_total             13058
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.09
_oxford_diffrn_Wilson_scale      0.11
_oxford_refine_ls_r_factor_ref   0.0651
_oxford_refine_ls_scale          2.846(15)
_oxford_reflns_number_all        13007
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt04162d2.cif
_cod_data_source_block           3_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        3586.88(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7045054
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT N    (  101 ,X'S,U'S)  UNTIL C    (   24 ) 
CONT H    ( 1221 ,X'S)  UNTIL H    ( 1051 ) 
CONT H    ( 2311 ,X'S)  UNTIL H    ( 1041 ) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) 
RIDE C   ( 214,X'S) H   (2141,X'S) 
RIDE C   ( 215,X'S) H   (2151,X'S) 
RIDE C   ( 216,X'S) H   (2161,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) 
RIDE C   ( 128,X'S) H   (1281,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) 
RIDE C   ( 203,X'S) H   (2031,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) 
RIDE C   ( 206,X'S) H   (2061,X'S) 
RIDE C   ( 222,X'S) H   (2221,X'S) 
RIDE C   ( 223,X'S) H   (2231,X'S) 
RIDE C   ( 224,X'S) H   (2241,X'S) 
RIDE C   ( 225,X'S) H   (2251,X'S) 
RIDE C   ( 226,X'S) H   (2261,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) 
END            
;
_iucr_refine_instructions_details_restraints
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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            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 101) TO H(1011) 
CONT N ( 101) TO H(1012) 
REST 0.038, 0.002 = H(1011,U[ISO]) 
REST 0.038, 0.002 = H(1012,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(103) TO N ( 101) TO H(1011) 
CONT C(103) TO N ( 101) TO H(1012) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 102) TO H(1021) 
CONT N ( 102) TO H(1022) 
REST 0.035, 0.002 = H(1021,U[ISO]) 
REST 0.035, 0.002 = H(1022,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(103) TO N ( 102) TO H(1021) 
CONT C(103) TO N ( 102) TO H(1022) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 104) TO H(1042) 
CONT N ( 104) TO H(1041) 
REST 0.030, 0.002 = H(1042,U[ISO]) 
REST 0.030, 0.002 = H(1041,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(106) TO N ( 104) TO H(1042) 
CONT C(106) TO N ( 104) TO H(1041) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 105) TO H(1052) 
CONT N ( 105) TO H(1051) 
REST 0.033, 0.002 = H(1052,U[ISO]) 
REST 0.033, 0.002 = H(1051,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(106) TO N ( 105) TO H(1052) 
CONT C(106) TO N ( 105) TO H(1051) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 121) TO H(1212) 
CONT N ( 121) TO H(1211) 
REST 0.037, 0.002 = H(1212,U[ISO]) 
REST 0.037, 0.002 = H(1211,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(123) TO N ( 121) TO H(1212) 
CONT C(123) TO N ( 121) TO H(1211) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 122) TO H(1221) 
CONT N ( 122) TO H(1222) 
REST 0.034, 0.002 = H(1221,U[ISO]) 
REST 0.034, 0.002 = H(1222,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(123) TO N ( 122) TO H(1221) 
CONT C(123) TO N ( 122) TO H(1222) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 124) TO H(1242) 
CONT N ( 124) TO H(1241) 
REST 0.037, 0.002 = H(1242,U[ISO]) 
REST 0.037, 0.002 = H(1241,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(126) TO N ( 124) TO H(1242) 
CONT C(126) TO N ( 124) TO H(1241) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 125) TO H(1252) 
CONT N ( 125) TO H(1251) 
REST 0.032, 0.002 = H(1252,U[ISO]) 
REST 0.032, 0.002 = H(1251,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(126) TO N ( 125) TO H(1252) 
CONT C(126) TO N ( 125) TO H(1251) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 231) TO H(2311) 
CONT O ( 231) TO H(2312) 
REST 0.063, 0.002 = H(2311,U[ISO]) 
REST 0.063, 0.002 = H(2312,U[ISO]) 
REM            H1-N-R2 
DIST 0.86, 0.02 = 
CONT N ( 7) TO H(71) 
REST 0.023, 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 0.025, 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) 
END                                                                             
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