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_7127857
_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 O4 P4 Rh, 2(F6 P), 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H77 Cl4 F12 Fe2 O4 P6 Rh'
_chemical_formula_weight         1512.34
_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                73.521(2)
_cell_angle_beta                 72.266(3)
_cell_angle_gamma                80.180(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9624(4)
_cell_length_b                   14.8814(4)
_cell_length_c                   18.4164(4)
_cell_measurement_reflns_used    19401
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.5210
_cell_measurement_theta_min      3.8170
_cell_volume                     3230.90(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_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 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.966
_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    -25.00  84.00   1.00   15.00    --   40.72 -99.00 150.00  109
  2  \w    -35.00  66.00   1.00   15.00    --   40.72 -57.00  30.00  101
  3  \w    -35.00  66.00   1.00   15.00    --   40.72 -57.00 -90.00  101
  4  \w    -42.00  27.00   1.00   15.00    --   40.72 -19.00 150.00   69
  5  \w     71.00 178.00   1.00   50.00    --  104.78  30.00 -90.00  107
  6  \w     71.00 178.00   1.00   50.00    --  104.78  30.00   0.00  107
  7  \w     71.00 178.00   1.00   50.00    --  104.78  30.00 150.00  107
  8  \w     29.00  71.00   1.00   50.00    --  104.78 -61.00 120.00   42
  9  \w     29.00  71.00   1.00   50.00    --  104.78 -61.00-120.00   42
 10  \w     76.00 178.00   1.00   50.00    --  104.78  45.00  60.00  102
 11  \w     18.00 145.00   1.00   50.00    --  104.78 -91.00-148.24  127
 12  \w     29.00  71.00   1.00   50.00    --  104.78 -61.00 -30.00   42
 13  \w     18.00 145.00   1.00   50.00    --  104.78 -91.00 -36.54  127
 14  \w     18.00 145.00   1.00   50.00    --  104.78 -91.00 118.41  127
 15  \w   -117.00 -10.00   1.00   15.00    --  -40.72 -57.00  60.00  107
 16  \w   -117.00 -10.00   1.00   15.00    --  -40.72 -57.00-180.00  107
 17  \w   -122.00  -6.00   1.00   15.00    --  -40.72 -77.00 150.00  116
 18  \w   -122.00  -6.00   1.00   15.00    --  -40.72 -77.00  30.00  116
 19  \w   -117.00 -10.00   1.00   15.00    --  -40.72 -57.00 -60.00  107
 20  \w     73.00 170.00   1.00   50.00    --  104.78  63.00-168.69   97
;
_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      0.0572836000
_diffrn_orient_matrix_UB_12      -0.0091281000
_diffrn_orient_matrix_UB_13      -0.0845042000
_diffrn_orient_matrix_UB_21      -0.1008138000
_diffrn_orient_matrix_UB_22      -0.0400611000
_diffrn_orient_matrix_UB_23      -0.0020604000
_diffrn_orient_matrix_UB_31      -0.0475186000
_diffrn_orient_matrix_UB_32      0.1003308000
_diffrn_orient_matrix_UB_33      -0.0326907000
_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  0.0322
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34376
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.928
_diffrn_reflns_theta_min         3.527
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.179
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         12257
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+1.9249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11123
_reflns_number_total             12257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08328c2.cif
_cod_data_source_block           jm396
_cod_depositor_comments
'Adding full bibliography for 7127856--7127859.cif.'
_cod_database_code               7127857
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H77 Cl4 F12 Fe2 O4 P6 Rh1'
_shelx_estimated_absorpt_t_max   0.499
_shelx_estimated_absorpt_t_min   0.298
_reflns_odcompleteness_completeness 99.14
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-C49 \\sim Cl4-C49 \\sim Cl2-C49 \\sim Cl1-C49
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl3 \\sim Cl2 \\sim Cl1: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F3A \\sim F4A \\sim F1A \\sim F6A \\sim F2A \\sim P5A \\sim F5A: within 1.9A
with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.9A
4. Others
 Fixed Sof: P5(0.9) Cl7(0.55) Cl1(0.7) Cl4(0.7) F4(0.9) F2(0.9) F3(0.9)
 F5(0.9) F1(0.9) F6(0.9) H49B(0.7) H49A(0.7) H49D(0.3) H49C(0.3) H50A(0.55)
 H50B(0.55) H50C(0.45) H50D(0.45) Cl2(0.3) Cl3(0.3) Cl6(0.45) P5A(0.1) F4A(0.1)
 F2A(0.1) F3A(0.1) F5A(0.1) F1A(0.1) F6A(0.1)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49B,H49A), C49(H49D,H49C), C50(H50A,H50B), C50(H50C,H50D)
5.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C12(H12), C31(H31), C15(H15)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C22(H22A,H22B,
 H22C), C41(H41A,H41B,H41C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C), C42(H42A,H42B,H42C), C10(H10A,H10B,H10C),
 C45(H45A,H45B,H45C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C19(H19A,H19B,H19C), C37(H37A,H37B,H37C), C17(H17A,H17B,H17C), C9(H9A,
 H9B,H9C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              10369
_shelx_hkl_checksum              83249
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.812