Hexa-<i>peri</i>-hexabenzocoronene decorated with an allenylidene ruthenium complex - almost a flyswatter.
Lorenz, Rebecca; Reger, David; Weller, Ruth; Jux, Norbert; Burzlaff, Nicolai; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13134–13141; doi:10.1039/d0dt02729d

data_7705405
_publ_section_title
;
 Hexa-<i>peri</i>-hexabenzocoronene decorated with an allenylidene
 ruthenium complex - almost a flyswatter.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13134
_journal_page_last               13141
_journal_paper_doi               10.1039/d0dt02729d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C112 H97 P2 Ru, 1(F6 P), 3.6(C3 H6 O)'
_chemical_formula_sum            'C122.8 H118.6 F6 O3.6 P3 Ru'
_chemical_formula_weight         1959.95
_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             2020-07-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-08-03 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                75.2303(17)
_cell_angle_beta                 70.2676(18)
_cell_angle_gamma                67.3264(19)
_cell_formula_units_Z            2
_cell_length_a                   14.9819(3)
_cell_length_b                   19.1809(4)
_cell_length_c                   20.0515(4)
_cell_measurement_reflns_used    46655
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1220
_cell_measurement_theta_min      2.8740
_cell_volume                     4952.68(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -87.00 -39.00   1.00   42.55    --  -11.17 154.00  -2.12   48
  2  \w    -13.00  86.00   1.00   42.55    --   11.64  38.00 -60.00   99
  3  \w    -63.00  36.00   1.00   42.55    --   11.64 -38.00   0.00   99
  4  \w    -20.00  53.00   1.00   42.55    --   11.64 -99.00   0.00   73
  5  \w    -20.00  53.00   1.00   42.55    --   11.64 -99.00-120.00   73
  6  \w    -61.00  40.00   1.00   42.55    --   11.64 -57.00 120.00  101
  7  \w    -13.00  86.00   1.00   42.55    --   11.64  38.00-180.00   99
  8  \w    -21.00  88.00   1.00   42.55    --   11.64  77.00  30.00  109
  9  \w    -88.00 -39.00   1.00   42.55    --  -11.17 155.00  72.21   49
 10  \w    -84.00  17.00   1.00   42.55    --  -11.17 -57.00  60.00  101
 11  \w    -68.00 -24.00   1.00   42.55    --  -11.17 126.00 -54.56   44
 12  \w    -87.00 -39.00   1.00   42.55    --  -11.17 154.00 150.57   48
 13  \w    -87.00 -39.00   1.00   42.55    --  -11.17 154.00-166.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258447000
_diffrn_orient_matrix_UB_12      0.0217528000
_diffrn_orient_matrix_UB_13      -0.0284218000
_diffrn_orient_matrix_UB_21      0.0464127000
_diffrn_orient_matrix_UB_22      -0.0255244000
_diffrn_orient_matrix_UB_23      0.0061541000
_diffrn_orient_matrix_UB_31      0.0038356000
_diffrn_orient_matrix_UB_32      -0.0227007000
_diffrn_orient_matrix_UB_33      -0.0244214000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            122139
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             2054
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1576
_refine_ls_number_reflns         20211
_refine_ls_number_restraints     2393
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+7.2482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16792
_reflns_number_total             20211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02729d2.cif
_cod_data_source_block           buni170628b_jl
_cod_depositor_comments          'Adding full bibliography for 7705405.cif.'
_cod_original_cell_volume        4952.66(19)
_cod_original_formula_sum        'C122.80 H118.60 F6 O3.60 P3 Ru'
_cod_database_code               7705405
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H Ru P F O'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C92B-C91B \\sim C96B-C91B \\sim C96B-C95B \\sim C95B-C94B \\sim C94B-C93B
\\sim C93B-C92B
 with sigma of 0.02
 C55A-C58A \\sim C55A-C57A \\sim C55A-C56A \\sim C56B-C55B \\sim C57B-C55B
\\sim C58B-C55B
 with sigma of 0.02
 C55B-C11 \\sim C55A-C11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C202 \\sim F4C \\sim P3C \\sim F6C \\sim F2C \\sim F1C \\sim F5C \\sim F3C
\\sim C201 \\sim C203 \\sim O202: within 4A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 4A
O192 \\sim C192 \\sim C193 \\sim C191: within 4A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 4A
C172 \\sim O172 \\sim C173 \\sim C171 \\sim F5A \\sim F1A \\sim F2A \\sim F6A
\\sim F3A \\sim F4A \\sim P3A \\sim P3B \\sim F1B \\sim F2B \\sim F6B \\sim F3B
\\sim F5B \\sim F4B: within 4A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 4A
O192 \\sim C192 \\sim C193 \\sim C191 \\sim H19A \\sim H19B \\sim H19C \\sim
H19D \\sim H19E \\sim H19F: within 4A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 4A
C44 \\sim C45 \\sim C43 \\sim C46: within 4A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 4A
C173 \\sim C183 \\sim C182 \\sim C172 \\sim O172 \\sim O182 \\sim C171 \\sim
C181: within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
4A
C93A \\sim C94A \\sim C94B \\sim C93B \\sim C92A \\sim C92B \\sim C95B \\sim
C95A \\sim C96A \\sim C96B \\sim C91A \\sim C91B: within 4A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 4A
C81A \\sim C81B \\sim C86B \\sim C86A \\sim C85A \\sim C85B \\sim C84B \\sim
C84A \\sim C83B \\sim C83A \\sim C82B \\sim C82A: within 4A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 4A
C56A \\sim C56B \\sim C57A \\sim C57B \\sim C58A \\sim C58B \\sim C55A \\sim
C55B: within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
4A
Uanis(C44) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C56A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C96A, C91A, C92A, C91A, C92A, C93A, C94A, C95A, C96A, C192, O192, C191, C193,
 P1, C81B, C81A, C82A, C82B, C86B, C56A, C55A, C11, C58A, C57A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C152)=Sof(O152)=Sof(C151)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C153)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(O162)=Sof(C161)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C162)=Sof(C163)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(1)
 Sof(C91A)=Sof(C92A)=Sof(H92A)=Sof(C93A)=Sof(H93A)=Sof(C94A)=Sof(H94A)=
 Sof(C95A)=Sof(H95A)=Sof(C96A)=Sof(H96A)=Sof(C85A)=Sof(H85A)=Sof(C84A)=
 Sof(H84A)=Sof(C83A)=Sof(H83A)=Sof(C82A)=Sof(H82A)=Sof(C81A)=Sof(C86A)=
 Sof(H86A)=Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C56A)=Sof(H56D)=
 Sof(H56E)=Sof(H56F)=Sof(C55A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(2)
 Sof(C55B)=Sof(C81B)=Sof(C82B)=Sof(H82B)=Sof(C58B)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=Sof(C57B)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C91B)=Sof(C92B)=
 Sof(H92B)=Sof(C83B)=Sof(H83B)=Sof(C56B)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C84B)=Sof(H84B)=Sof(C96B)=Sof(H96B)=Sof(C95B)=Sof(H95B)=Sof(C86B)=
 Sof(H86B)=Sof(C85B)=Sof(H85B)=Sof(C93B)=Sof(H93B)=Sof(C94B)=Sof(H94B)=FVAR(2)
 Sof(O182)=Sof(C182)=Sof(C181)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C183)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(3)
 Sof(C172)=Sof(O172)=Sof(C173)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C171)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=FVAR(3)
 Fixed Sof: F4C(0.4) F6C(0.4) F2C(0.4) P3C(0.4) F1C(0.4) F5C(0.4) F3C(0.4)
 P3A(0.3) F3A(0.3) F5A(0.3) F2A(0.3) F1A(0.3) F6A(0.3) F4A(0.3) P3B(0.3)
 F2B(0.3) F6B(0.3) F1B(0.3) F4B(0.3) F5B(0.3) F3B(0.3) C201(0.6) H20A(0.6)
 H20B(0.6) H20C(0.6) C202(0.6) C203(0.6) H20D(0.6) H20E(0.6) H20F(0.6) O202(0.6)
6.a Free rotating group:
 P3A(F3A,F5A,F2A,F1A,F6A,F4A), P3B(F2B,F6B,F1B,F4B,F5B,F3B)
6.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C21(H21), C42(H42), C5(H5), C2(H2), C36(H36), C7(H7), C10(H10),
 C29(H29), C113(H113), C34(H34), C76(H76), C105(H105), C12(H12), C40(H40),
 C72(H72), C114(H114), C146(H146), C116(H116), C107(H107), C112(H112),
 C106(H106), C73(H73), C104(H104), C115(H115), C126(H126), C132(H132),
 C103(H103), C145(H145), C142(H142), C125(H125), C75(H75), C133(H133), C74(H74),
  C144(H144), C82B(H82B), C143(H143), C134(H134), C136(H136), C124(H124),
 C92B(H92B), C83B(H83B), C122(H122), C135(H135), C123(H123), C84B(H84B),
 C96B(H96B), C95B(H95B), C86B(H86B), C85B(H85B), C93B(H93B), C94B(H94B),
 C92A(H92A), C93A(H93A), C94A(H94A), C95A(H95A), C96A(H96A), C85A(H85A),
 C84A(H84A), C83A(H83A), C82A(H82A), C86A(H86A)
6.c Fitted hexagon refined as free rotating group:
 C85A(C84A,C83A,C82A,C81A,C86A)
6.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C60(H60A,H60B,H60C), C48(H48A,H48B,H48C), C53(H53A,H53B,
 H53C), C49(H49A,H49B,H49C), C61(H61A,H61B,H61C), C50(H50A,H50B,H50C), C52(H52A,
 H52B,H52C), C54(H54A,H54B,H54C), C58B(H58A,H58B,H58C), C45(H45A,H45B,H45C),
 C57B(H57A,H57B,H57C), C56B(H56A,H56B,H56C), C46(H46A,H46B,H46C), C44(H44A,H44B,
 H44C), C173(H17A,H17B,H17C), C171(H17D,H17E,H17F), C193(H19A,H19B,H19C),
 C161(H16A,H16B,H16C), C163(H16D,H16E,H16F), C191(H19D,H19E,H19F), C151(H15A,
 H15B,H15C), C153(H15D,H15E,H15F), C201(H20A,H20B,H20C), C203(H20D,H20E,H20F),
 C181(H18A,H18B,H18C), C183(H18D,H18E,H18F), C57A(H57D,H57E,H57F), C56A(H56D,
 H56E,H56F), C58A(H58D,H58E,H58F)
;
_shelx_res_checksum              90954
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.782