Study and modular synthesis of unsymmetrical bis(phosphino)pyrrole ligands.
Fokwa, Hilary D.; Vidlak, Julia F.; Weinberg, Sophie C.; Duplessis, Isaiah D.; Schley, Nathan D.; Johnson, Miles W.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9957–9960; doi:10.1039/d0dt02063j

data_7704844
_publ_section_title
;
 Study and modular synthesis of unsymmetrical bis(phosphino)pyrrole
 ligands.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9957
_journal_page_last               9960
_journal_paper_doi               10.1039/d0dt02063j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C22 H27 Cl2 N P2 Pt'
_chemical_formula_sum            'C22 H27 Cl2 N P2 Pt'
_chemical_formula_weight         633.37
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.565(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9874(2)
_cell_length_b                   16.6163(3)
_cell_length_c                   14.1086(3)
_cell_measurement_reflns_used    14762
_cell_measurement_temperature    99.96(12)
_cell_measurement_theta_max      29.6330
_cell_measurement_theta_min      3.1510
_cell_volume                     2320.99(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.96(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.899
_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    -52.00  87.00   1.00   15.00    --   17.49   0.00-150.00  139
  2  \w     -9.00  85.00   1.00   15.00    --   17.49  77.00  60.00   94
  3  \w      1.00  85.00   1.00   15.00    --   17.49  57.00   0.00   84
  4  \w     35.00  90.00   1.00   15.00    --   17.49 178.00 120.00   55
  5  \w    -69.00 -21.00   1.00   15.00    --  -17.73 122.00  88.00   48
  6  \w     35.00  60.00   1.00   15.00    --   17.49 178.00 -90.00   25
  7  \w     -1.00  87.00   1.00   15.00    --   17.49  38.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0385086000
_diffrn_orient_matrix_UB_12      0.0286049000
_diffrn_orient_matrix_UB_13      0.0293409000
_diffrn_orient_matrix_UB_21      -0.0413825000
_diffrn_orient_matrix_UB_22      0.0313592000
_diffrn_orient_matrix_UB_23      -0.0217449000
_diffrn_orient_matrix_UB_31      -0.0440750000
_diffrn_orient_matrix_UB_32      -0.0044761000
_diffrn_orient_matrix_UB_33      0.0351667000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28248
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.948
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.422
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1232
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         6054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0165P)^2^+0.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5548
_reflns_number_total             6054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02063j2.cif
_cod_data_source_block           scw-ii-31
_cod_depositor_comments
'Adding full bibliography for 7704840--7704845.cif.'
_cod_database_code               7704844
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C22H27Cl2NP2Pt
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              76433
_olex2_date_sample_data_collection 2019-04-23
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_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 2.978
_oxdiff_exptl_absorpt_empirical_full_min 0.557