A hydrogen bonded Co(ii) coordination complex and a triply interpenetrating 3-D manganese(ii) coordination polymer from diaza crown ether with dibenzoate sidearms
Liao, Liang; Ingram, Conrad W.; Bacsa, John; Zhang, Z. John; Dinadayalane, Tandabany; CrystEngComm 18 (2016) 2425–; doi:10.1039/C6CE00360E

data_7224504
_publ_section_title
;
 A hydrogen bonded Co(ii) coordination complex and a triply
 interpenetrating 3-D manganese(ii) coordination polymer from diaza crown
 ether with dibenzoate sidearms
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2425
_journal_paper_doi               10.1039/C6CE00360E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.13(C192 H224 Mn8 N16 O48), 2(H2 O)'
_chemical_formula_sum            'C24 H32 Mn N2 O8'
_chemical_formula_weight         531.45
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-04-15
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr  9 2013 14:10:59, GUI svn.r4458)
;
_audit_update_record
;
2015-08-19 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.046(4)
_cell_length_b                   9.0309(10)
_cell_length_c                   16.4592(18)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      37.694
_cell_measurement_theta_min      2.471
_cell_volume                     4912.0(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type
'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15648
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.751
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.785
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.7485.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       prism
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.888
_exptl_crystal_size_mid          0.619
_exptl_crystal_size_min          0.318
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0928P)^2^+0.2252P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.626
_reflns_number_gt                4627
_reflns_number_total             4964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00360e2.cif
_cod_data_source_block           fdd2
_cod_depositor_comments
'Adding full bibliography for 7224504--7224506.cif.'
_cod_original_cell_volume        4912.0(9)
_cod_database_code               7224504
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C6-H6 = C4-H4 = C3-H3
 0.999 with sigma of 0.005
 C7-H7
 0.999 with sigma of 0.005
 C10-H10A = C10-H10B
 0.999 with sigma of 0.005
 H1WA-O1W = O1W-H1WB
 0.995 with sigma of 0.02
 H1WA-O1W = O1W-H1WB
 0.995 with sigma of 0.02
 O1-H1WA
 1.81 with sigma of 0.02
 H1WA-H1WB
 1.61 with sigma of 0.04
 H1WA-H1WB
 1.61 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(H6) = Uiso(H4) = Uiso(H3)
Uiso(H10B) = Uiso(H10A)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C8(H8B,H8A), C12(H12A,H12B), C9(H9A,H9B)
;
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.623
_shelxl_version_number           2012-9