Carbyne decorated porphyrins.
Frogley, Benjamin J.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12390–12400; doi:10.1039/d0dt02809f

data_7705250
_publ_section_title
;
 Carbyne decorated porphyrins.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12390
_journal_page_last               12400
_journal_paper_doi               10.1039/d0dt02809f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C116 H114 Au4 B4 Cl4 N28 O8 W4'
_chemical_formula_sum            'C116 H114 Au4 B4 Cl4 N28 O8 W4'
_chemical_formula_weight         3736.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-08 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                86.793(6)
_cell_angle_beta                 67.571(8)
_cell_angle_gamma                80.675(6)
_cell_formula_units_Z            1
_cell_length_a                   15.2352(12)
_cell_length_b                   15.6101(10)
_cell_length_c                   16.9339(15)
_cell_measurement_reflns_used    2569
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      39.4570
_cell_measurement_theta_min      5.5100
_cell_volume                     3673.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     14.00  74.00   1.00   90.00    --   42.11 -98.00 -93.00   60
  2  \w    -19.00  57.00   1.00   90.00    --   42.11 -38.00-150.00   76
  3  \w     14.00 114.00   1.00   90.00    --   42.11  19.00-150.00  100
  4  \w      7.00  75.00   1.00   90.00    --   42.11 -99.00   0.00   68
  5  \w     32.00  60.00   1.00   90.00    --   42.11-125.00  90.00   28
  6  \w     68.00  96.00   1.00   90.00    --   42.11-125.00  90.00   28
  7  \w    -19.00  69.00   1.00   90.00    --   42.11 -77.00 150.00   88
  8  \w     40.00  72.00   1.00   90.00    --   42.11  57.00   0.00   32
  9  \w     62.00 114.00   1.00   90.00    --   42.11  19.00  60.00   52
 10  \w     32.00  78.00   1.00   90.00    --   42.11  57.00 -30.00   46
 11  \w    -15.00  18.00   1.00   90.00    --   42.11 -77.00  60.00   33
 12  \w     30.00  68.00   1.00   90.00    --   42.11 -77.00  60.00   38
 13  \w   -110.00 -52.00   1.00   90.00    --  -42.81 -57.00  90.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0413761000
_diffrn_orient_matrix_UB_12      0.0119392000
_diffrn_orient_matrix_UB_13      -0.0705967000
_diffrn_orient_matrix_UB_21      -0.0911553000
_diffrn_orient_matrix_UB_22      -0.0350447000
_diffrn_orient_matrix_UB_23      0.0603748000
_diffrn_orient_matrix_UB_31      -0.0472292000
_diffrn_orient_matrix_UB_32      0.0929091000
_diffrn_orient_matrix_UB_33      0.0325267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9229
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        40.220
_diffrn_reflns_theta_max         40.220
_diffrn_reflns_theta_min         3.943
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       plate
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     779
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0916P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2920
_reflns_number_total             4364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02809f2.cif
_cod_data_source_block           Compound_6
_cod_depositor_comments
'Adding full bibliography for 7705247--7705250.cif.'
_cod_original_cell_volume        3673.4(5)
_cod_database_code               7705250
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C116 H114 Au4 B4 Cl4 N28 O8 W4'
_reflns_odcompleteness_completeness 97.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B2-H2
 1.15 with sigma of 0.02
 B1-H1
 1.15 with sigma of 0.02
 C57-C56
 1.5 with sigma of 0.02
 C56-C55
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C1)
4. Rigid body (RIGU) restrains
 C34, C43, C39, C49, B2, C33, B1, C29, C10, C25, N10, C57, C52, C26, C56, C37,
 C27, C55, C1, C38, C11, C54, C024, C21, C35, C15, C45, C16, C44, O1, N14, C47,
 C20, C46, N4, W1, C14, C40, C6, N3, C3, Au2, C12, O4, N13, Au1, O2, O3, N12,
 Cl2, Cl1, N7, N9, N1, N5, C17, C13, C42, C18, C24, N6, C48, C19, C4, C9, N8,
 W2, C31, C32, C30, C51, C8, C36, C22, N11, C23, C53, C2, C28, C41, C50, C5, N2,
  C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H13(0.5) H14(0.5)
6.a Ternary CH refined with riding coordinates and stretchable bonds:
 B1(H1), B2(H2)
6.b Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C52(H52A,H52B,H52C), C57(H57A,H57B,H57C)
6.c Aromatic/amide H refined with riding coordinates:
 N13(H13), N14(H14), C19(H19), C20(H20), C10(H10), C23(H23), C7(H7), C6(H6),
 C11(H11), C22(H22), C3(H3), C15(H15), C16(H16), C4(H4), C27(H27), C46(H46),
 C50(H50), C32(H32), C37(H37), C55(H55)
6.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C53(H53A,H53B,H53C), C35(H35A,H35B,
 H35C), C024(H02A,H02B,H02C), C34(H34A,H34B,H34C), C29(H29A,H29B,H29C),
 C25(H25A,H25B,H25C), C39(H39A,H39B,H39C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91486
_shelx_fab_checksum              94556
_ins_header
;
TITL exp_1009_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  15.235166  15.610077  16.933913  86.7925  67.5705  80.6752
ZERR    1.00   0.001173   0.000969   0.001495   0.0061   0.0077   0.0058
LATT  1
SFAC C H B N O Cl W Au
UNIT 116.00 114.00 4.00 28.00 8.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.418
_oxdiff_exptl_absorpt_empirical_full_min 0.600