PNN' & P<sub>2</sub>NN' ligands via reductive amination with phosphine aldehydes: synthesis and base-metal coordination chemistry.
Gradiski, Matthew V.; Tsui, Brian T. H.; Lough, Alan J.; Morris, Robert H.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2150–2159; doi:10.1039/c8dt04058c

data_7048653
_publ_section_title
;
 PNN' &amp; P<sub>2</sub>NN' ligands via reductive amination with
 phosphine aldehydes: synthesis and base-metal coordination chemistry.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2150
_journal_page_last               2159
_journal_paper_doi               10.1039/c8dt04058c
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H29 Cl2 Co N2 P, 0.5(C5 H12)'
_chemical_formula_sum            'C21.5 H35 Cl2 Co N2 P'
_chemical_formula_weight         482.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2019-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.8587(4)
_cell_length_b                   19.4737(9)
_cell_length_c                   30.7593(14)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.27
_cell_measurement_theta_min      2.87
_cell_volume                     4707.3(4)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            96373
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.364
_diffrn_reflns_theta_max         67.364
_diffrn_reflns_theta_min         2.685
_diffrn_source                   'Bruker ImuS with multi-layer optics'
_exptl_absorpt_coefficient_mu    8.508
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.490(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0213P)^2^+4.5181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                7443
_reflns_number_total             8368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04058c2.cif
_cod_data_source_block           8_d1834_b_sq
_cod_depositor_comments
'Adding full bibliography for 7048646--7048653.cif.'
_cod_original_formula_sum        'C21.50 H35 Cl2 Co N2 P'
_cod_database_code               7048653
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.172
_shelx_estimated_absorpt_t_max   0.848
_shelx_res_checksum              12788
_shelx_fab_checksum              32974