Diphosphene with a phosphineborane tether and its rhodium complex.
Tsurusaki, Akihiro; Takechi, Shingo; Kamikawa, Ken; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2929–2936; doi:10.1039/d3dt03509c

data_7714672
_publ_section_title
;
 Diphosphene with a phosphineborane tether and its rhodium complex.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2929
_journal_page_last               2936
_journal_paper_doi               10.1039/d3dt03509c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C53 H76 B P3 Rh, B F4, 2(C2 H4 Cl2), [C2H4Cl2]'
_chemical_formula_sum            'C59 H88 B2 Cl6 F4 P3 Rh'
_chemical_formula_weight         1303.43
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_chemical_temperature_decomposition 424.15
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-11-30 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                97.4885(16)
_cell_angle_beta                 96.6648(17)
_cell_angle_gamma                101.8517(17)
_cell_formula_units_Z            2
_cell_length_a                   10.4512(2)
_cell_length_b                   13.8345(3)
_cell_length_c                   23.1447(4)
_cell_measurement_reflns_used    23307
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      75.7040
_cell_measurement_theta_min      1.8680
_cell_volume                     3211.79(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
'<i>SHELXL-2014/7</i> and <i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45374
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.986
_diffrn_reflns_theta_min         1.946
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloroethane/diisopropyl ether'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         13105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0677P)^2^+6.7178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11689
_reflns_number_total             13105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03509c2.cif
_cod_data_source_block           RhPP
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_temperature_decomposition' since the value had been given
as '151 \%C, decomp.'. The value '151 \%C, decomp.' was changed to
'424.15' -- it was converted from degrees Celsius (C) to kelvins (K).

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7714671--7714672.cif.
;
_cod_original_cell_volume        3211.78(11)
_cod_database_code               7714672
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.436
_shelx_estimated_absorpt_t_max   0.769
_oxdiff_exptl_absorpt_empirical_full_min 0.577
_oxdiff_exptl_absorpt_empirical_full_max 2.322
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              22790
_shelx_fab_checksum              33273