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_7045052
_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 H24 N4 Ni O8, 2(C8 H12 N4), 2 (H2 O)'
_chemical_formula_sum            'C64 H52 N12 Ni O10'
_chemical_formula_weight         1207.90
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.86990(10)
_cell_length_b                   24.1347(2)
_cell_length_c                   24.7076(2)
_cell_measurement_reflns_used    31637
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.6
_cell_measurement_theta_min      4.37
_cell_volume                     6481.84(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            104624
_diffrn_reflns_theta_full        74.007
_diffrn_reflns_theta_max         74.007
_diffrn_reflns_theta_min         2.559
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.79
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0690
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6541
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.0007745
_refine_ls_shift/su_mean         0.0000711
_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: 
 0.363E+04 0.617E+04 0.386E+04 0.163E+04 364. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2099
_refine_ls_wR_factor_gt          0.2069
_refine_ls_wR_factor_ref         0.2099
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                5971
_reflns_number_total             6567
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      0.21
_oxford_refine_ls_r_factor_ref   0.0762
_oxford_refine_ls_scale          1.780(17)
_oxford_reflns_number_all        6541
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt04162d2.cif
_cod_data_source_block           3_4
_cod_depositor_comments
'Adding full bibliography for 7045051--7045058.cif.'
_cod_original_cell_volume        6481.84(5)
_cod_original_sg_symbol_H-M      'P n n a '
_cod_original_formula_sum        'C64 H52 N12 Ni1 O10'
_cod_database_code               7045052
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT O    (    1 ,X'S,U'S)  UNTIL NI   (    1 ) 
CONT H    (  552 ,X'S)  UNTIL H    (  511 ) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
END      
;
_iucr_refine_instructions_details_restraints
;                                                                  
NO 
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 ( 51) TO H(512) 
CONT N ( 51) TO H(511) 
REST 0.052, 0.002 = H(512,U[ISO]) 
REST 0.052, 0.002 = H(511,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(53) TO N ( 51) TO H(512) 
CONT C(53) TO N ( 51) TO H(511) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 52) TO H(522) 
CONT N ( 52) TO H(521) 
REST 0.034, 0.002 = H(522,U[ISO]) 
REST 0.034, 0.002 = H(521,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(53) TO N ( 52) TO H(522) 
CONT C(53) TO N ( 52) TO H(521) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 54) TO H(541) 
CONT N ( 54) TO H(542) 
REST 0.027, 0.002 = H(541,U[ISO]) 
REST 0.027, 0.002 = H(542,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(56) TO N ( 54) TO H(541) 
CONT C(56) TO N ( 54) TO H(542) 
REM            H2-N-R 
DIST 0.86, 0.02 = 
CONT N ( 55) TO H(552) 
CONT N ( 55) TO H(551) 
REST 0.026, 0.002 = H(552,U[ISO]) 
REST 0.026, 0.002 = H(551,U[ISO]) 
ANGLE 120.0, 2.0 = 
CONT C(56) TO N ( 55) TO H(552) 
CONT C(56) TO N ( 55) TO H(551) 
REM       H ON O-HETRO ATOM 
DIST 0.82, 0.02 = 
CONT O ( 101) TO H(1012) 
CONT O ( 101) TO H(1011) 
REST 0.092, 0.002 = H(1012,U[ISO]) 
REST 0.092, 0.002 = H(1011,U[ISO]) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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