Structure, resolution and chirooptical analysis of stable lanthanide complexes of a pyridylmethylphosphinate triazacyclonane ligand
James W. Walton; Lorenzo Di Bari; David Parker; Gennaro Pescitelli; Horst Puschmann; Dmitry S. Yufit; Chem.Commun. 47 (2011) 12289–; doi:10.1039/c1cc14904k

data_7107039
_publ_section_title
;
 Structure, resolution and chirooptical analysis of stable lanthanide
 complexes of a pyridylmethylphosphinate triazacyclonane ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              12289
_journal_paper_doi               10.1039/c1cc14904k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C42 H42 N6 Nd O6 P3'
_chemical_formula_sum            'C42 H42 N6 Nd O6 P3'
_chemical_formula_weight         963.97
_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_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-07-18
_audit_creation_method
;
Olex2 1.1-beta
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.584(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1667(5)
_cell_length_b                   22.6624(6)
_cell_length_c                   15.9874(6)
_cell_measurement_reflns_used    14367
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      33.0681
_cell_measurement_theta_min      2.5732
_cell_volume                     5073.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
1 omega -102.00 -75.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -27.1651 179.0000 30.0000 54

2 omega -99.00 -8.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -27.1651 -38.0000 -120.0000 182

3 omega -87.00 41.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -27.1651 0.0000 -90.0000 256

4 omega 65.00 103.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- 27.9463 179.0000 -30.0000 76

5 omega -97.00 3.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- -27.1651 -77.0000 150.0000 200

6 omega -42.00 56.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- 27.9463 -77.0000 30.0000 196

7 omega 56.00 104.00 0.5000 20.0000
omega____ theta____ kappa____ phi______ frames
- 27.9463 179.0000 60.0000 96
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      0.0351170000
_diffrn_orient_matrix_UB_12      -0.0179086000
_diffrn_orient_matrix_UB_13      -0.0067230000
_diffrn_orient_matrix_UB_21      -0.0054946000
_diffrn_orient_matrix_UB_22      -0.0214155000
_diffrn_orient_matrix_UB_23      0.0299567000
_diffrn_orient_matrix_UB_31      -0.0360264000
_diffrn_orient_matrix_UB_32      -0.0141227000
_diffrn_orient_matrix_UB_33      -0.0370206000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56906
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr 6 2011,09:17:13)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.454
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         13469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                10869
_reflns_number_total             13469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14904k.txt
_cod_data_source_block           NdL3_11srv130e
_cod_database_code               7107039
_chemical_oxdiff_formula         'C42 H42 N6 O6 P3 Nb1'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.93