Mono- and dimeric complexes of an asymmetric heterotopic P,CNHC,pyr ligand.
Bouché, Mathilde; Mordan, Michael; Kariuki, Benson M.; Coles, Simon J.; Christensen, Jeppe; Newman, Paul D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13347–13360; doi:10.1039/c6dt02476a

data_7040061
_publ_section_title
;
 Mono- and dimeric complexes of an asymmetric heterotopic P,CNHC,pyr
 ligand.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13347
_journal_page_last               13360
_journal_paper_doi               10.1039/c6dt02476a
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C35 H38 Cl N3 Ni P, F6 P'
_chemical_formula_sum            'C35 H38 Cl F6 N3 Ni P2'
_chemical_formula_weight         770.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.045(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9383(3)
_cell_length_b                   19.4448(3)
_cell_length_c                   17.0362(4)
_cell_measurement_reflns_used    18071
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4620
_cell_measurement_theta_min      1.9870
_cell_volume                     3445.26(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 14.286
_diffrn_detector_type            'Rigaku HG Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    '0.1 mm Confocal mirrors, HF Varimax'
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32767
_diffrn_reflns_point_group_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.694
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.615
_diffrn_reflns_theta_min         1.636
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'FR-E+ SuperBright rotating anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       leaf
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 3247 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         13427
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+3.8260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.486
_reflns_Friedel_fraction_full    0.632
_reflns_Friedel_fraction_max     0.466
_reflns_number_gt                11096
_reflns_number_total             13427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02476a2.cif
_cod_data_source_block           cmpd10
_cod_depositor_comments
'Adding full bibliography for 7040057--7040062.cif.'
_cod_original_cell_volume        3445.25(15)
_cod_database_code               7040061
_shelx_res_checksum              17316
_shelx_hkl_checksum              83787