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_7704845
_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 Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.5 H28 Cl3 N P2 Pd'
_chemical_formula_weight         587.15
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-30
_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                 93.0442(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.03203(16)
_cell_length_b                   9.55406(6)
_cell_length_c                   18.39924(10)
_cell_measurement_reflns_used    28170
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.2950
_cell_measurement_theta_min      2.7990
_cell_volume                     4920.73(5)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3012
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -108.00  -7.00   1.00    1.00    --  -36.45 -19.00  60.00  101
  2  \w   -106.00 -18.00   1.00    1.00    --  -36.45 -38.00-120.00   88
  3  \w    -53.00  31.00   1.00    1.00    --  -36.45  57.00-120.00   84
  4  \w      1.00  75.00   1.00    1.00    --   36.45 -99.00-180.00   74
  5  \w    -31.00  63.00   1.00    1.00    --   36.45 -77.00-120.00   94
  6  \w     40.00 126.00   1.00    1.39    --  108.65 -45.00  90.00   86
  7  \w    100.00 178.00   1.00    1.39    --  108.65 111.00   0.00   78
  8  \w     39.00 115.00   1.00    1.39    --  108.65-111.00 -90.00   76
  9  \w     91.00 177.00   1.00    1.39    --  108.65  45.00  90.00   86
 10  \w    100.00 178.00   1.00    1.39    --  108.65 111.00-120.00   78
 11  \w     91.00 177.00   1.00    1.39    --  108.65  45.00-120.00   86
 12  \w     37.00 147.00   1.00    1.39    --  108.65 -15.00  30.00  110
 13  \w     41.00 135.00   1.00    1.39    --  108.65 -77.00 -90.00   94
 14  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00-150.00   94
 15  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00   0.00   94
 16  \w    -55.00  33.00   1.00    1.00    --  -36.45  38.00  60.00   88
 17  \w     39.00 115.00   1.00    1.39    --  108.65-111.00  90.00   76
 18  \w     82.00 176.00   1.00    1.39    --  108.65  77.00  30.00   94
 19  \w     91.00 176.00   1.00    1.39    --  108.65  61.00 120.00   85
 20  \w     91.00 177.00   1.00    1.39    --  108.65  45.00-150.00   86
 21  \w     70.00 178.00   1.00    1.39    --  108.65  15.00 -30.00  108
 22  \w     87.00 178.00   1.00    1.39    --  108.65  30.00-180.00   91
 23  \w   -104.00 -34.00   1.00    1.00    --  -36.45 -77.00  90.00   70
 24  \w    -90.00  -2.00   1.00    1.00    --  -36.45 125.00  60.00   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      -0.0131356000
_diffrn_orient_matrix_UB_12      0.0710692000
_diffrn_orient_matrix_UB_13      0.0714036000
_diffrn_orient_matrix_UB_21      0.0420031000
_diffrn_orient_matrix_UB_22      -0.0751722000
_diffrn_orient_matrix_UB_23      0.0409099000
_diffrn_orient_matrix_UB_31      0.0330650000
_diffrn_orient_matrix_UB_32      0.1235579000
_diffrn_orient_matrix_UB_33      -0.0162551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47966
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.360
_diffrn_reflns_theta_min         3.157
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.388
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.142
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.101
_refine_diff_density_max         2.345
_refine_diff_density_min         -1.916
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0369P)^2^+16.7708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9359
_reflns_number_total             9646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02063j2.cif
_cod_data_source_block           scw-ii-30a
_cod_depositor_comments
'Adding full bibliography for 7704840--7704845.cif.'
_cod_original_cell_volume        4920.72(5)
_cod_original_formula_sum        'C22.50 H28 Cl3 N P2 Pd'
_cod_database_code               7704845
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C22.5H28Cl3NP2Pd
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8), C5B(H5B), C8B(H8B)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B)
2.c 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), C2B(H2B), C3B(H3B), C4B(H4B),
  C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C18B(H18B),
 C19B(H19B), C20B(H20B), C21B(H21B), C22B(H22B)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,
 H10F)
;
_shelx_res_checksum              42444
_olex2_date_sample_data_collection 2019-04-24
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.850