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_7704841
_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         'C29 H34 Cl N Ni P2'
_chemical_formula_sum            'C29 H34 Cl N Ni P2'
_chemical_formula_weight         552.67
_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             2020-01-30
_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                 96.599(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7452(6)
_cell_length_b                   10.5763(4)
_cell_length_c                   29.5471(11)
_cell_measurement_reflns_used    11581
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8230
_cell_measurement_theta_min      3.0030
_cell_volume                     5508.6(3)
_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 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.915
_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     35.00  90.00   1.00   30.00    --   17.49 178.00 150.00   55
  2  \w    -52.00  36.00   1.00   30.00    --   17.49 -38.00   0.00   88
  3  \w     35.00  90.00   1.00   30.00    --   17.49 178.00  60.00   55
  4  \w     35.00  90.00   1.00   30.00    --   17.49 178.00-120.00   55
  5  \w    -50.00  34.00   1.00   30.00    --   17.49 -57.00-120.00   84
  6  \w    -20.00  56.00   1.00   30.00    --   17.49 -99.00-150.00   76
  7  \w    -20.00  56.00   1.00   30.00    --   17.49 -99.00 -90.00   76
  8  \w    -85.00 -18.00   1.00   30.00    --  -17.73 -57.00 120.00   67
  9  \w    -85.00   9.00   1.00   30.00    --  -17.73 -77.00 -30.00   94
;
_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      -0.0167153000
_diffrn_orient_matrix_UB_12      0.0509676000
_diffrn_orient_matrix_UB_13      -0.0131457000
_diffrn_orient_matrix_UB_21      0.0323998000
_diffrn_orient_matrix_UB_22      0.0034592000
_diffrn_orient_matrix_UB_23      -0.0119509000
_diffrn_orient_matrix_UB_31      -0.0170216000
_diffrn_orient_matrix_UB_32      -0.0434593000
_diffrn_orient_matrix_UB_33      -0.0163797000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            79588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.979
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.637
_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    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         14653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0254P)^2^+6.7011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10595
_reflns_number_total             14653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02063j2.cif
_cod_data_source_block           mwj-2-018
_cod_depositor_comments
'Adding full bibliography for 7704840--7704845.cif.'
_cod_database_code               7704841
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C29H34ClNNiP2
_reflns_odcompleteness_completeness 99.91
_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:
 C12(H12), C15(H15), C12A(H12A), C15A(H15A)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C9A(H9A), C10A(H10A),
 C11A(H11A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A),
 C25A(H25A), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C7A(H7AA,H7AB,H7AC), C13A(H13D,H13E,H13F),
 C14A(H14D,H14E,H14F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
;
_shelx_res_checksum              31750
_olex2_date_sample_data_collection 2020-01-30
_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 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.589