From a P<sub>4</sub> butterfly scaffold to <i>cyclo</i>- and <i>catena</i>-P<sub>4</sub> units.
Müller, Julian; Balázs, Gábor; Scheer, Manfred; Chemical communications (Cambridge, England) 57 (2021) 2257–2260; doi:10.1039/d0cc08328c

data_7127856
_publ_section_title
;
 From a P<sub>4</sub> butterfly scaffold to <i>cyclo</i>- and
 <i>catena</i>-P<sub>4</sub> units.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2257
_journal_page_last               2260
_journal_paper_doi               10.1039/d0cc08328c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C48 H72 Fe2 O4 P4 Ru, 2(F6 P)'
_chemical_formula_sum            'C48 H72 F12 Fe2 O4 P6 Ru'
_chemical_formula_weight         1339.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-26
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2021-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0919(2)
_cell_length_b                   14.4515(2)
_cell_length_c                   40.1739(6)
_cell_measurement_reflns_used    33967
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      32.2320
_cell_measurement_theta_min      3.3566
_cell_volume                     5852.26(17)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.920
_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   -101.00  15.00   0.50   25.00    --  -19.91 -77.00 -60.00  232
  2  \w    -96.00  11.00   0.50   25.00    --  -19.91 -57.00  30.00  214
  3  \w   -101.00  15.00   0.50   25.00    --  -19.91 -77.00-180.00  232
  4  \w     53.00 111.00   0.50   25.00    --   21.47-178.00 -60.00  116
  5  \w     57.00 101.00   0.50   25.00    --   21.47 178.00-150.00   88
  6  \w     53.00 111.00   0.50   25.00    --   21.47-178.00  90.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0123544000
_diffrn_orient_matrix_UB_12      -0.0081934000
_diffrn_orient_matrix_UB_13      -0.0172765000
_diffrn_orient_matrix_UB_21      0.0561909000
_diffrn_orient_matrix_UB_22      0.0271010000
_diffrn_orient_matrix_UB_23      -0.0035503000
_diffrn_orient_matrix_UB_31      0.0404990000
_diffrn_orient_matrix_UB_32      -0.0401066000
_diffrn_orient_matrix_UB_33      0.0011364000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            79434
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.463
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       plate
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.249
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         19438
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0342P)^2^+4.8390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16675
_reflns_number_total             19438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08328c2.cif
_cod_data_source_block           jm256
_cod_depositor_comments
'Adding full bibliography for 7127856--7127859.cif.'
_cod_database_code               7127856
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H72 F12 Fe2 O4 P6 Ru1'
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.661
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P6-F7 \\sim P6-F8 \\sim P6-F12 \\sim P6-F9 \\sim P6-F10 \\sim P6-F11
 with sigma of 0.02
 F7-F8 \\sim F7-F10 \\sim F9-F8 \\sim F9-F10 \\sim F11-F7 \\sim F11-F8 \\sim
F11-F9 \\sim F11-F10 \\sim F12-F7
 \\sim F12-F8 \\sim F12-F9 \\sim F12-F10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P6 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2.5A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2.5A
P6 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18: within 2.5A
with sigma of 0.02 and sigma for terminal atoms of 0.02 within 2.5A
4. Others
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Fixed Sof: H8A(0.56459) H8B(0.43541) C9A(0.43541) H9AA(0.43541) H9AB(0.43541)
 H9AC(0.43541) C10(0.56459) H10A(0.56459) H10B(0.56459) H10C(0.56459)
5.a Ternary CH refined with riding coordinates:
 C8(H8A), C8(H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C34(H34), C31(H31), C5(H5), C6(H6), C2(H2), C3(H3)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C),
 C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C41(H41A,H41B,
 H41C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C9(H9A,
 H9B,H9C), C9A(H9AA,H9AB,H9AC), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              35182
_shelx_hkl_checksum              53995
_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 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.853