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_7704843
_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         'C44 H54 Cl2 Cu2 N2 P4'
_chemical_formula_sum            'C44 H54 Cl2 Cu2 N2 P4'
_chemical_formula_weight         932.75
_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
_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                75.136(3)
_cell_angle_beta                 73.244(3)
_cell_angle_gamma                62.259(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6486(3)
_cell_length_b                   10.1503(3)
_cell_length_c                   13.6583(5)
_cell_measurement_reflns_used    17302
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2010
_cell_measurement_theta_min      3.3950
_cell_volume                     1121.76(7)
_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      100.01(10)
_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 0.987
_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    -63.00  31.00   1.00    1.00    --  -36.45  77.00   0.00   94
  2  \w    -66.00  35.00   1.00    1.00    --  -36.45  19.00   0.00  101
  3  \w   -106.00 -49.00   1.00    1.00    --  -36.45-160.00 -48.00   57
  4  \w    -53.00  31.00   1.00    1.00    --  -36.45  57.00 120.00   84
  5  \w   -106.00 -18.00   1.00    1.00    --  -36.45 -38.00-180.00   88
  6  \w     23.00  90.00   1.00    1.00    --   36.45-125.00-150.00   67
  7  \w     23.00  90.00   1.00    1.00    --   36.45-125.00 -60.00   67
  8  \w     23.00  90.00   1.00    1.00    --   36.45-125.00 120.00   67
  9  \w     39.00 109.00   1.00    1.00    --  108.65 -94.00 -90.00   70
 10  \w     37.00 147.00   1.00    1.00    --  108.65 -15.00-180.00  110
 11  \w     42.00 127.00   1.00    1.00    --  108.65 -61.00 120.00   85
 12  \w     39.00 109.00   1.00    1.00    --  108.65 -94.00  30.00   70
 13  \w     40.00 126.00   1.00    1.00    --  108.65 -45.00 150.00   86
 14  \w     40.00 126.00   1.00    1.00    --  108.65 -45.00 -30.00   86
 15  \w    100.00 178.00   1.00    1.00    --  108.65 111.00 -60.00   78
 16  \w     70.00 178.00   1.00    1.00    --  108.65  15.00-150.00  108
 17  \w     39.00 115.00   1.00    1.00    --  108.65-111.00-120.00   76
 18  \w     39.00 109.00   1.00    1.00    --  108.65 -94.00 -60.00   70
 19  \w     39.00 115.00   1.00    1.00    --  108.65-111.00 150.00   76
 20  \w     40.00 126.00   1.00    1.00    --  108.65 -45.00-120.00   86
 21  \w     39.00 130.00   1.00    1.00    --  108.65 -30.00   0.00   91
 22  \w     57.00 151.00   1.00    1.00    --  108.65 178.00-180.00   94
 23  \w   -104.00 -20.00   1.00    1.00    --  -36.45 -57.00 -90.00   84
 24  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00   0.00   94
 25  \w    -55.00  33.00   1.00    1.00    --  -36.45  38.00-120.00   88
 26  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00 -90.00   94
 27  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00-180.00   94
 28  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00  90.00   94
 29  \w     70.00 178.00   1.00    1.00    --  108.65  15.00  30.00  108
 30  \w     87.00 178.00   1.00    1.00    --  108.65  30.00 150.00   91
 31  \w     87.00 178.00   1.00    1.00    --  108.65  30.00 -30.00   91
 32  \w     87.00 178.00   1.00    1.00    --  108.65  30.00  60.00   91
 33  \w     82.00 176.00   1.00    1.00    --  108.65  77.00-150.00   94
 34  \w     70.00 178.00   1.00    1.00    --  108.65  15.00 120.00  108
 35  \w     82.00 176.00   1.00    1.00    --  108.65  77.00-180.00   94
 36  \w     87.00 178.00   1.00    1.00    --  108.65  30.00 -60.00   91
 37  \w     82.00 176.00   1.00    1.00    --  108.65  77.00  90.00   94
 38  \w     82.00 176.00   1.00    1.00    --  108.65  77.00   0.00   94
 39  \w     82.00 176.00   1.00    1.00    --  108.65  77.00 -30.00   94
 40  \w     70.00 178.00   1.00    1.00    --  108.65  15.00 -60.00  108
 41  \w   -106.00 -40.00   1.00    1.00    --  -36.45 -38.00 -60.00   66
 42  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00  30.00   94
 43  \w   -104.00 -10.00   1.00    1.00    --  -36.45 -77.00 150.00   94
 44  \w     20.00 104.00   1.00    1.00    --   36.45  57.00 120.00   84
 45  \w     18.00 106.00   1.00    1.00    --   36.45  38.00   0.00   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      0.0174322000
_diffrn_orient_matrix_UB_12      0.0311112000
_diffrn_orient_matrix_UB_13      0.0994264000
_diffrn_orient_matrix_UB_21      0.0480775000
_diffrn_orient_matrix_UB_22      0.1268630000
_diffrn_orient_matrix_UB_23      -0.0631928000
_diffrn_orient_matrix_UB_31      -0.1767752000
_diffrn_orient_matrix_UB_32      0.1138910000
_diffrn_orient_matrix_UB_33      0.0170825000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21063
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.410
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.858
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.323
_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    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.6582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4294
_reflns_number_total             4381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02063j2.cif
_cod_data_source_block           idd-ii-63
_cod_depositor_comments
'Adding full bibliography for 7704840--7704845.cif.'
_cod_database_code               7704843
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C44H54Cl2Cu2N2P4
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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              27238
_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 1.100
_oxdiff_exptl_absorpt_empirical_full_min 0.905