Aspects of the coordination chemistry of rac-trans-1,2-diphosphinocyclohexane and the preparation of reinforced 9aneP3 and 9anePN2 macrocycles.
Edwards, Peter G.; Kariuki, Benson M.; Newman, Paul D.; Tallis, Huw A.; Williams, Craig; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15532–15545; doi:10.1039/c4dt02239d

data_7032169
_publ_section_title
;
 Aspects of the coordination chemistry of
 rac-trans-1,2-diphosphinocyclohexane and the preparation of reinforced
 9aneP3 and 9anePN2 macrocycles.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15532
_journal_page_last               15545
_journal_paper_doi               10.1039/c4dt02239d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C21 H29 Mn N2 O3 P, P F6, C H2 Cl2'
_chemical_formula_sum            'C22 H31 Cl2 F6 Mn N2 O3 P2'
_chemical_formula_weight         673.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.1450(10)
_cell_angle_beta                 73.3360(10)
_cell_angle_gamma                72.4180(10)
_cell_formula_units_Z            4
_cell_length_a                   14.2290(2)
_cell_length_b                   14.4430(3)
_cell_length_c                   16.8230(4)
_cell_measurement_reflns_used    8990
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.23
_cell_volume                     3064.39(11)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21717
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_correction_T_min  0.7476
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0056(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13925
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+4.1706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1930
_reflns_number_gt                8990
_reflns_number_total             13925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02239d1.cif
_cod_data_source_block           cmpd16c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7032169--7032173.cif.
;
_cod_original_cell_volume        3064.40(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7032169