Transition metal complexes of the pyridylphosphine ligand o-C6H4(CH2PPy2)2.
Vaughan, Teresa F.; Spencer, John L.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16826–16837; doi:10.1039/c6dt02041k

data_7040761
_publ_section_title
;
 Transition metal complexes of the pyridylphosphine ligand
 o-C6H4(CH2PPy2)2.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16826
_journal_page_last               16837
_journal_paper_doi               10.1039/c6dt02041k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H36 Ir N4 P2, C24 H20 B'
_chemical_formula_sum            'C60 H56 B Ir N4 P2'
_chemical_formula_weight         1098.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-04-23 deposited with the CCDC.
2016-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                84.324(2)
_cell_angle_beta                 88.2410(17)
_cell_angle_gamma                79.2307(17)
_cell_formula_units_Z            2
_cell_length_a                   9.38338(15)
_cell_length_b                   14.6521(4)
_cell_length_c                   17.9389(5)
_cell_measurement_reflns_used    16193
_cell_measurement_temperature    285.10(10)
_cell_measurement_theta_max      76.0820
_cell_measurement_theta_min      4.1280
_cell_volume                     2410.85(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      285.10(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9853
_diffrn_measured_fraction_theta_max 0.9853
_diffrn_measurement_details
;
  1 omega  -25.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000   37.0000  -60.0000 40

  2 omega   31.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9338 -125.0000 -120.0000 53

  3 omega   36.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 54

  4 omega   67.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -60.0000 57

  5 omega  135.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -60.0000 42

  6 omega  145.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 28

  7 omega  151.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  111.0000   30.0000 26

  8 omega  101.00  175.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  111.0000  -60.0000 74

  9 omega  129.00  167.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  111.0000 -120.0000 38

 10 omega  112.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  178.0000 -120.0000 27

 11 omega   78.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  178.0000 -120.0000 32

 12 omega   93.00  128.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000    0.0000 35

 13 omega   65.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000    0.0000 26

 14 omega   99.00  125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -30.0000 26

 15 omega   73.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000    0.0000 43

 16 omega   58.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000  -30.0000 50

 17 omega   52.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -30.0000 36

 18 omega   45.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 62

 19 omega   85.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000 -150.0000 31

 20 omega   43.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 41

 21 omega   39.00  156.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000  -60.0000 117

 22 omega   63.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -117.0000  132.0000 54

 23 omega   44.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000   30.0000 51

 24 omega   44.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -111.0000   60.0000 72

 25 omega   44.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 36

 26 omega   31.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 57

 27 omega   31.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9338 -125.0000   30.0000 57

 28 omega   32.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 63

 29 omega   46.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 25

 30 omega -115.00  -68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000 -161.0000  -19.0000 47

 31 omega -119.00   37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000    0.0000   90.0000 156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0248745000
_diffrn_orient_matrix_UB_12      -0.0018104000
_diffrn_orient_matrix_UB_13      -0.0851698000
_diffrn_orient_matrix_UB_21      -0.0167172000
_diffrn_orient_matrix_UB_22      -0.1031079000
_diffrn_orient_matrix_UB_23      0.0063668000
_diffrn_orient_matrix_UB_31      -0.1644274000
_diffrn_orient_matrix_UB_32      0.0304061000
_diffrn_orient_matrix_UB_33      -0.0124354000
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23896
_diffrn_reflns_theta_full        76.5422
_diffrn_reflns_theta_max         76.54
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.332
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.5126
_exptl_crystal_description       plate
_exptl_crystal_F_000             1106.8858
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.1768
_refine_diff_density_min         -1.6280
_refine_diff_density_rms         0.1154
_refine_ls_d_res_high            0.7927
_refine_ls_d_res_low             14.3291
_refine_ls_goodness_of_fit_ref   1.0420
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    106
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0420
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.8957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                9540
_reflns_number_total             9988
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt02041k2.cif
_cod_data_source_block           TVE
_cod_depositor_comments
'Adding full bibliography for 7040761--7040764.cif.'
_cod_database_code               7040761
_chemical_oxdiff_formula         'C60 H56 B1 N4 O9 P2 Ir1'
_chemical_oxdiff_usercomment     'Teresa John S/ Vic/ 9028'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C29(H29), C34(H34), C30(H30), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36a,H36b), C1(H1a,H1b), C35(H35a,H35b), C33(H33a,H33b), C8(H8a,H8b),
 C32(H32a,H32b)
2.c Aromatic/amide H refined with riding coordinates:
 C48(H48), C21(H21), C20(H20), C3(H3), C45(H45), C57(H57), C27(H27), C58(H58),
 C46(H46), C13(H13), C54(H54), C16(H16), C59(H59), C28(H28), C17(H17), C47(H47),
  C25(H25), C44(H44), C15(H15), C56(H56), C38(H38), C60(H60), C18(H18),
 C50(H50), C53(H53), C52(H52), C5(H5), C11(H11), C6(H6), C26(H26), C42(H42),
 C4(H4), C10(H10), C39(H39), C23(H23), C51(H51), C12(H12), C40(H40), C22(H22),
 C41(H41)
;
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method n-hexane/dichloromethane