#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/58/2105873.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2105873
loop_
_publ_author_name
'Rood, Jeffrey A.'
'Huttenstine, Ashley L.'
'Schmidt, Zachery A.'
'White, Michael R.'
'Oliver, Allen G.'
_publ_section_title
;
 Linear alkaline earth metal phosphinate coordination polymers: synthesis
 and structural characterization
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              602
_journal_page_last               607
_journal_paper_doi               10.1107/S2052520614004247
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C30 H34 Ba N2 O6 P2'
_chemical_formula_sum            'C30 H34 Ba N2 O6 P2'
_chemical_formula_weight         717.85
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6068(7)
_cell_length_b                   6.0118(4)
_cell_length_c                   26.6405(19)
_cell_measurement_reflns_used    9198
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.4540
_cell_measurement_theta_min      2.4585
_cell_volume                     1523.50(19)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 - ApexII CCD Diffractometer'
_diffrn_measurement_method       'φ and ω 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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22314
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.453
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Blessing, R.H. (1995) Acta Cryst. A51, 33-38.
Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0159P)²+1.3613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0414
_reflns_number_gt                2694
_reflns_number_total             3153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ry5058sup1.cif
_cod_data_source_block           jr65b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105873
_cod_database_fobs_code          2105873
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ba Ba1 0.5000 0.0000 0.0000 0.00985(5) Uani d S 1 2
P P1 0.55484(4) 0.49164(8) 0.099263(16) 0.01148(9) Uani d . 1 1
O O2 0.57640(14) -0.3101(2) 0.06681(5) 0.0188(3) Uani d . 1 1
O O1 0.23805(14) -0.1655(2) 0.00507(5) 0.0229(3) Uani d . 1 1
C C15 0.43435(19) 0.4291(3) 0.18693(7) 0.0175(4) Uani d . 1 1
H H15 0.4743 0.2846 0.1869 0.021 Uiso calc R 1 1
C C9 0.78006(19) 0.2039(3) 0.13199(7) 0.0167(4) Uani d . 1 1
H H9 0.7277 0.0920 0.1125 0.020 Uiso calc R 1 1
C C3 0.1305(2) -0.6693(4) 0.06122(9) 0.0321(5) Uani d . 1 1
H H3A 0.1895 -0.7573 0.0415 0.048 Uiso calc R 1 1
H H3B 0.0338 -0.7254 0.0553 0.048 Uiso calc R 1 1
H H3C 0.1669 -0.6814 0.0974 0.048 Uiso calc R 1 1
C C1 0.22361(19) -0.3630(3) 0.01658(7) 0.0195(4) Uani d . 1 1
H H1 0.2823 -0.4694 0.0036 0.023 Uiso calc R 1 1
C C2 0.0430(2) -0.2832(4) 0.06845(9) 0.0323(5) Uani d . 1 1
H H2A 0.0854 -0.2501 0.1033 0.049 Uiso calc R 1 1
H H2B -0.0498 -0.3505 0.0688 0.049 Uiso calc R 1 1
H H2C 0.0330 -0.1453 0.0487 0.049 Uiso calc R 1 1
N N1 0.13248(17) -0.4370(3) 0.04566(6) 0.0199(4) Uani d . 1 1
C C4 0.72381(18) 0.4165(3) 0.13468(6) 0.0117(3) Uani d . 1 1
C C7 0.9891(2) 0.3164(3) 0.18651(7) 0.0200(4) Uani d . 1 1
H H7 1.0799 0.2826 0.2039 0.024 Uiso calc R 1 1
C C5 0.80156(19) 0.5770(3) 0.16431(7) 0.0161(4) Uani d . 1 1
H H5 0.7635 0.7217 0.1669 0.019 Uiso calc R 1 1
C C6 0.9337(2) 0.5282(3) 0.19005(7) 0.0201(4) Uani d . 1 1
H H6 0.9858 0.6390 0.2100 0.024 Uiso calc R 1 1
C C8 0.9130(2) 0.1547(3) 0.15783(7) 0.0209(4) Uani d . 1 1
H H8 0.9512 0.0098 0.1557 0.025 Uiso calc R 1 1
C C10 0.45226(18) 0.5782(3) 0.14816(7) 0.0131(4) Uani d . 1 1
C C13 0.2986(2) 0.7000(4) 0.22532(7) 0.0248(5) Uani d . 1 1
H H13 0.2464 0.7420 0.2516 0.030 Uiso calc R 1 1
C C14 0.3584(2) 0.4906(4) 0.22559(7) 0.0243(4) Uani d . 1 1
H H14 0.3476 0.3890 0.2521 0.029 Uiso calc R 1 1
C C11 0.3928(2) 0.7891(3) 0.14870(7) 0.0190(4) Uani d . 1 1
H H11 0.4056 0.8933 0.1229 0.023 Uiso calc R 1 1
C C12 0.3146(2) 0.8479(4) 0.18695(8) 0.0258(5) Uani d . 1 1
H H12 0.2720 0.9907 0.1866 0.031 Uiso calc R 1 1
O O3 0.49009(13) 0.2861(2) 0.07381(5) 0.0166(3) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Ba1 O2 3_655 . 180.00(8)
O2 Ba1 O3 3_655 3_655 89.62(4)
O2 Ba1 O3 . 3_655 90.38(4)
O2 Ba1 O3 3_655 . 90.38(4)
O2 Ba1 O3 . . 89.62(4)
O3 Ba1 O3 3_655 . 180.00(6)
O2 Ba1 O1 3_655 . 96.94(4)
O2 Ba1 O1 . . 83.06(4)
O3 Ba1 O1 3_655 . 85.89(4)
O3 Ba1 O1 . . 94.11(4)
O2 Ba1 O1 3_655 3_655 83.06(4)
O2 Ba1 O1 . 3_655 96.94(4)
O3 Ba1 O1 3_655 3_655 94.11(4)
O3 Ba1 O1 . 3_655 85.89(4)
O1 Ba1 O1 . 3_655 180.00(8)
O3 P1 O2 . 1_565 118.30(8)
O3 P1 C10 . . 109.13(8)
O2 P1 C10 1_565 . 108.51(8)
O3 P1 C4 . . 108.28(8)
O2 P1 C4 1_565 . 108.10(8)
C10 P1 C4 . . 103.52(8)
P1 O2 Ba1 1_545 . 155.47(8)
C1 O1 Ba1 . . 119.86(12)
C14 C15 C10 . . 120.55(19)
C4 C9 C8 . . 120.26(18)
O1 C1 N1 . . 124.94(19)
C1 N1 C2 . . 120.61(17)
C1 N1 C3 . . 121.60(18)
C2 N1 C3 . . 117.33(17)
C9 C4 C5 . . 118.84(17)
C9 C4 P1 . . 121.74(14)
C5 C4 P1 . . 119.40(14)
C8 C7 C6 . . 120.29(18)
C6 C5 C4 . . 120.94(18)
C5 C6 C7 . . 119.59(18)
C7 C8 C9 . . 120.07(18)
C11 C10 C15 . . 118.96(17)
C11 C10 P1 . . 122.21(14)
C15 C10 P1 . . 118.82(14)
C12 C13 C14 . . 120.08(18)
C13 C14 C15 . . 119.85(19)
C10 C11 C12 . . 120.17(19)
C13 C12 C11 . . 120.37(19)
P1 O3 Ba1 . . 145.23(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ba1 O2 3_655 2.6111(12)
Ba1 O2 . 2.6111(12)
Ba1 O3 3_655 2.6241(12)
Ba1 O3 . 2.6241(12)
Ba1 O1 . 2.7268(13)
Ba1 O1 3_655 2.7268(13)
P1 O3 . 1.5019(13)
P1 O2 1_565 1.5035(13)
P1 C10 . 1.8160(18)
P1 C4 . 1.8168(18)
O2 P1 1_545 1.5035(13)
O1 C1 . 1.239(2)
C15 C14 . 1.393(3)
C15 C10 . 1.396(3)
C9 C4 . 1.393(3)
C9 C8 . 1.395(3)
C3 N1 . 1.458(3)
C1 N1 . 1.324(2)
C2 N1 . 1.452(3)
C4 C5 . 1.395(3)
C7 C8 . 1.381(3)
C7 C6 . 1.388(3)
C5 C6 . 1.387(3)
C10 C11 . 1.391(3)
C13 C12 . 1.380(3)
C13 C14 . 1.383(3)
C11 C12 . 1.394(3)
