Manganese(II) and cobalt(II) complexes of 1,4-bis(diphenylphosphinoyl)butane
Lees, Anthony M. J.; Platt, Andrew W. G.; Acta Crystallographica Section C 65 (2009) m10–m13; doi:10.1107/S010827010804033X

data_2016930
_publ_section_title
;
 Manganese(II) and cobalt(II) complexes of
 1,4-bis(diphenylphosphinoyl)butane
;
_journal_coeditor_code           SF3094
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m10
_journal_page_last               m13
_journal_paper_doi               10.1107/S010827010804033X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Mn (C2 H6 O)2 (C28 H28 O2 P2) (H2 O)2] (N O3)2 , C28 H28 O2 P2'
_chemical_formula_moiety
'C32 H44 Mn1 O6 P2 2+ , 2N O3 - , 2C14 H14 O P'
_chemical_formula_sum            'C60 H72 Mn N2 O14 P4'
_chemical_formula_weight         1224.02
_chemical_name_systematic
;
<i>catena</i>-poly[[[diaquadiethanolmanganese(II)]-\m-1,4-
bis(diphenylphosphinoyl)butane-\k^2^O:O'] dinitrate
1,4-bis(diphenylphosphinoyl)butane solvate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.9000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4134(3)
_cell_length_b                   10.3270(3)
_cell_length_c                   22.1028(6)
_cell_measurement_reflns_used    7147
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1
_cell_volume                     2995.89(14)
_computing_cell_refinement
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998)
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
WinGX publication routines (Farrugia, 1999) and enCIFer (Allen <i>et
al.</i>,  2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
'Bruker Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40734
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut plate'
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0438P)^2^+3.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                5673
_reflns_number_total             6856
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3094.cif
_cod_data_source_block           I
_cod_original_cell_volume        2995.88(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C60 H72 Mn1 N2 O14 P4'
_cod_database_code               2016930
_cod_database_fobs_code          2016930