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_7040762
_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         'C29 H27 Cl N4 P2 Pt, 2(C H2 Cl2)'
_chemical_formula_sum            'C31 H31 Cl5 N4 P2 Pt'
_chemical_formula_weight         893.92
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-22
_audit_creation_method
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Olex2 1.2-dev
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-09-03 deposited with the CCDC.
2016-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.905(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4790(4)
_cell_length_b                   10.3594(4)
_cell_length_c                   22.7769(8)
_cell_measurement_reflns_used    6071
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      33.7900
_cell_measurement_theta_min      2.9780
_cell_volume                     3416.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   52.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.7502 -178.0000 -180.0000 69

  2 omega  -40.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.7502  -19.0000  150.0000 128

  3 omega    0.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       35.7502   57.0000  -90.0000 75
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0084850000
_diffrn_orient_matrix_UB_12      0.0616853000
_diffrn_orient_matrix_UB_13      -0.0124032000
_diffrn_orient_matrix_UB_21      0.0451268000
_diffrn_orient_matrix_UB_22      0.0001816000
_diffrn_orient_matrix_UB_23      -0.0121851000
_diffrn_orient_matrix_UB_31      -0.0171142000
_diffrn_orient_matrix_UB_32      -0.0296903000
_diffrn_orient_matrix_UB_33      -0.0258297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            33117
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.658
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method
'Vapour diffusion of hexane into CH2Cl2 solution'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.939
_refine_diff_density_min         -3.229
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0411P)^2^+12.1721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5169
_reflns_number_total             6624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02041k2.cif
_cod_data_source_block           tvbmo
_cod_depositor_comments
'Adding full bibliography for 7040761--7040764.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7040762
_reflns_odcompleteness_completeness 87.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     37.48
_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. Shared sites
{C51, Cl1}
{Cl2, C52}
3. Uiso/Uaniso restraints and constraints
Uanis(C51) = Uanis(Cl1)
Uanis(Cl2) = Uanis(C52)
4. Others
 Sof(Cl1)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=1-FVAR(1)
 Sof(Cl2)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4AA(H4AA), C6AA(H6AA), C6(H6), C20(H20), C5AA(H5AA), C4(H4),
 C2AA(H2AA), C3AA(H3AA), C9AA(H9AA), C9(H9), C10(H10), C11(H11), C5(H5),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19)
5.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              34182
_shelx_fab_checksum              38696
_olex2_submission_special_instructions 'No special instructions were received'