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_7127858
_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         'C47 H73 Fe2 O3 P4 Ru, F6 P, 0.7(C4 H8 O1)'
_chemical_formula_sum            'C49.8 H78.6 F6 Fe2 O3.7 P5 Ru'
_chemical_formula_weight         1218.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-08-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-21 deposited with the CCDC.	2021-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5480(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.66252(20)
_cell_length_b                   16.39571(14)
_cell_length_c                   20.2876(3)
_cell_measurement_reflns_used    33628
_cell_measurement_temperature    123.01(13)
_cell_measurement_theta_max      73.8960
_cell_measurement_theta_min      3.4390
_cell_volume                     6008.67(12)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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   -115.00 -21.00   1.00    5.00    --  -44.08 -38.00 150.00   94
  2  \w    -50.00  27.00   1.00    5.00    --  -44.08  38.00   0.00   77
  3  \w    -50.00  27.00   1.00    5.00    --  -44.08  38.00 120.00   77
  4  \w    -50.00  27.00   1.00    5.00    --  -44.08  38.00  90.00   77
  5  \w     32.00  91.00   1.00   20.00    --  104.50 -30.00 -90.00   59
  6  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00 120.00   62
  7  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00  60.00   62
  8  \w     32.00  91.00   1.00   20.00    --  104.50 -30.00   0.00   59
  9  \w     33.00 135.00   1.00   20.00    --  104.50 -77.00   0.00  102
 10  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00-180.00   62
 11  \w     82.00 173.00   1.00   20.00    --  104.50  45.00 -60.00   91
 12  \w     33.00 121.00   1.00   20.00    --  104.50-125.00   0.00   88
 13  \w   -113.00 -20.00   1.00    5.00    --  -44.08 -57.00  90.00   93
 14  \w   -113.00 -20.00   1.00    5.00    --  -44.08 -57.00 -60.00   93
 15  \w   -113.00 -20.00   1.00    5.00    --  -44.08 -57.00  30.00   93
 16  \w     82.00 173.00   1.00   20.00    --  104.50  45.00-120.00   91
 17  \w     81.00 177.00   1.00   20.00    --  104.50  30.00-180.00   96
 18  \w     82.00 173.00   1.00   20.00    --  104.50  45.00   0.00   91
 19  \w     82.00 111.00   1.00   20.00    --  104.50  45.00 120.00   29
 20  \w     68.00 178.00   1.00   20.00    --  104.50  15.00  90.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0767398000
_diffrn_orient_matrix_UB_12      -0.0342782000
_diffrn_orient_matrix_UB_13      0.0004085000
_diffrn_orient_matrix_UB_21      0.0362319000
_diffrn_orient_matrix_UB_22      -0.0805381000
_diffrn_orient_matrix_UB_23      0.0305050000
_diffrn_orient_matrix_UB_31      0.0084864000
_diffrn_orient_matrix_UB_32      0.0341917000
_diffrn_orient_matrix_UB_33      0.0722868000
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.387
_diffrn_reflns_theta_min         2.446
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.558
_exptl_absorpt_correction_T_max  0.544
_exptl_absorpt_correction_T_min  0.292
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         12096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0497P)^2^+3.7939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11464
_reflns_number_total             12096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08328c2.cif
_cod_data_source_block           jm203_2
_cod_depositor_comments
'Adding full bibliography for 7127856--7127859.cif.'
_cod_original_cell_volume        6008.68(11)
_cod_original_formula_sum        'C49.80 H78.60 F6 Fe2 O3.70 P5 Ru'
_cod_database_code               7127858
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H73 F6 Fe2 O4 P5 Ru1'
_shelx_estimated_absorpt_t_max   0.496
_shelx_estimated_absorpt_t_min   0.195
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Fixed Sof: O4(0.7) C51(0.7) H51A(0.7) H51B(0.7) C50(0.7) H50A(0.7) H50B(0.7)
 C49(0.7) H49A(0.7) H49B(0.7) C48(0.7) H48A(0.7) H48B(0.7)
3.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C50(H50A,H50B), C49(H49A,H49B), C48(H48A,H48B)
3.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C33(H33), C12(H12), C15(H15)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C45(H45A,H45B,H45C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C41(H41A,H41B,
 H41C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C23(H23A,H23B,H23C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42120
_shelx_hkl_checksum              52850
_shelx_fab_checksum              85473
_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 2.310
_oxdiff_exptl_absorpt_empirical_full_min 0.605