Porphyrin-Polyyne [3]- and [5]Rotaxanes.
Kohn, Daniel R.; Movsisyan, Levon D.; Thompson, Amber L.; Anderson, Harry L.; Organic letters 19 (2017) 348–351; doi:10.1021/acs.orglett.6b03528

data_1545005
_publ_section_title
;
 Porphyrin-Polyyne [3]- and [5]Rotaxanes.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              348
_journal_page_last               351
_journal_paper_doi               10.1021/acs.orglett.6b03528
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C301 H348 N8 O17 Zn1'
_chemical_formula_sum            'C301 H348 N8 O17 Zn'
_chemical_formula_weight         4415.49
_chemical_melting_point          ?
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-11-14
_audit_creation_method           CRYSTALS_ver_14.61_build_6019
_cell_angle_alpha                90
_cell_angle_beta                 96.0619(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.7209(5)
_cell_length_b                   19.3373(2)
_cell_length_c                   50.4748(7)
_cell_measurement_reflns_used    60958
_cell_measurement_temperature    100
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     30787.9(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device
;
CrystalLogic Kappa (3 circle)
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            246020
_diffrn_reflns_theta_full        21.246
_diffrn_reflns_theta_max         22.476
_diffrn_reflns_theta_min         1.547
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clear_intense_red
_exptl_crystal_density_diffrn    0.953
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9504
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
; 
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5933
_refine_ls_number_reflns         52640
_refine_ls_number_restraints     18794
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.1236
_refine_ls_shift/su_max          0.0165890
_refine_ls_shift/su_mean         0.0000485
_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: 
 0.664E+04 0.113E+05 0.710E+04 0.310E+04 771. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3567
_refine_ls_wR_factor_gt          0.3163
_refine_ls_wR_factor_ref         0.3567
_reflns_limit_h_max              34
_reflns_limit_h_min              -35
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              55
_reflns_limit_l_min              -55
_reflns_number_gt                40509
_reflns_number_total             77776
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.90
_oxford_diffrn_Wilson_scale      1.26
_oxford_refine_ls_r_factor_ref   0.1407
_oxford_refine_ls_scale          1.616(6)
_oxford_reflns_number_all        52640
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title DIA0244
_cod_data_source_file            ol6b03528_si_002.cif
_cod_data_source_block           Zn-P3Ra
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1545005.cif.
;
_cod_original_sg_symbol_H-M      'P c '
_cod_original_formula_sum        'C301 H348 N8 O17 Zn1'
_cod_database_code               1545005
_platon_squeeze_void_probe_radius 1.20