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_7127859
_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 H73 Fe2 Ir O4 P4, 2(C H2 Cl2), 2(F6 P)'
_chemical_formula_sum            'C50 H77 Cl4 F12 Fe2 Ir O4 P6'
_chemical_formula_weight         1601.63
_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
_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                73.4890(10)
_cell_angle_beta                 72.3460(10)
_cell_angle_gamma                80.0700(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9537(2)
_cell_length_b                   14.8742(2)
_cell_length_c                   18.4134(2)
_cell_measurement_reflns_used    58377
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      32.4320
_cell_measurement_theta_min      3.6780
_cell_volume                     3226.85(8)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.937
_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    -53.00  50.00   1.00   22.50    --   20.91 -57.00-120.00  103
  2  \w     -9.00  61.00   1.00   22.50    --   20.91 -94.00 113.00   70
  3  \w    -18.00  30.00   1.00   22.50    --   20.91  94.00-135.00   48
  4  \w    -58.00  55.00   1.00   22.50    --   20.91 -77.00   0.00  113
  5  \w    -46.00  57.00   1.00   22.50    --  -19.35  38.00-150.00  103
  6  \w    -95.00   7.00   1.00   22.50    --  -19.35 -38.00-150.00  102
  7  \w    -49.00  55.00   1.00   22.50    --  -19.35  57.00  30.00  104
  8  \w     -4.00  63.00   1.00   22.50    --   20.91 -99.00-180.00   67
  9  \w     -9.00  95.00   1.00   22.50    --   20.91  57.00 120.00  104
 10  \w     -9.00  95.00   1.00   22.50    --   20.91  57.00   0.00  104
 11  \w    -93.00   3.00   1.00   22.50    --  -19.35 -57.00 120.00   96
 12  \w     -4.00  63.00   1.00   22.50    --   20.91 -99.00 -60.00   67
 13  \w    -98.00 -17.00   1.00   22.50    --  -19.35 157.00 129.86   81
 14  \w    -95.00 -48.00   1.00   22.50    --  -19.35 153.00 -94.36   47
 15  \w    -90.00 -10.00   1.00   22.50    --  -19.35 146.00  30.26   80
;
_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      0.0360863000
_diffrn_orient_matrix_UB_12      0.0024343000
_diffrn_orient_matrix_UB_13      -0.0380314000
_diffrn_orient_matrix_UB_21      0.0040903000
_diffrn_orient_matrix_UB_22      -0.0497795000
_diffrn_orient_matrix_UB_23      0.0074011000
_diffrn_orient_matrix_UB_31      -0.0448629000
_diffrn_orient_matrix_UB_32      0.0034883000
_diffrn_orient_matrix_UB_33      -0.0154666000
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            124329
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.890
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.890
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.469
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.123
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         22599
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+1.7773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20785
_reflns_number_total             22599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08328c2.cif
_cod_data_source_block           jm249
_cod_depositor_comments
'Adding full bibliography for 7127856--7127859.cif.'
_cod_database_code               7127859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H77 Cl4 F12 Fe2 Ir1 O4 P6'
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.406
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl5-C50 \\sim Cl6-C50
 with sigma of 0.02
 Cl1-C49 \\sim Cl1A-C49A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl1 \\sim C49 \\sim Cl2 \\sim C49A \\sim Cl1A: within 1.9A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.9A
Cl4 \\sim Cl6 \\sim Cl5 \\sim C50: within 2A with sigma of 0.05 and sigma for
terminal atoms of 0.05 within 2A
4. Others
 Sof(Cl2A)=Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
 Fixed Sof: Cl6(0.6) Cl5(0.4) H50C(0.6) H50D(0.6) H50A(0.4) H50B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C50(H50C,H50D), C50(H50A,H50B), C49(H49A,H49B), C49A(H49C,H49D)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C31(H31), C34(H34)
5.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), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C),
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              47397
_shelx_hkl_checksum              97828
_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 1.251
_oxdiff_exptl_absorpt_empirical_full_min 0.823