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_7224505
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H32 Co N2 O8'
_chemical_formula_sum            'C24 H32 Co N2 O8'
_chemical_formula_weight         535.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-22
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.06.08 svn.r3188 for OlexSys, GUI svn.r5058)
;
_audit_update_record
;
2015-08-19 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 131.453(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7472(9)
_cell_length_b                   22.777(2)
_cell_length_c                   7.0903(7)
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.178
_cell_measurement_theta_min      2.928
_cell_volume                     1179.8(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4351
_diffrn_reflns_point_group_measured_fraction_full 0.702
_diffrn_reflns_point_group_measured_fraction_max 0.669
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.569
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0745 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.8469.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       prism
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.033(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2263
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.344
_reflns_Friedel_fraction_full    0.402
_reflns_Friedel_fraction_max     0.344
_reflns_number_gt                2072
_reflns_number_total             2263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00360e2.cif
_cod_data_source_block           92_58-67-co
_cod_depositor_comments
'Adding full bibliography for 7224504--7224506.cif.'
_cod_database_code               7224505
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H) groups
2. Restrained distances
 O6-H6
 0.995 with sigma of 0.005
 O5-H5
 0.995 with sigma of 0.005
 H5_$1-H5
 1.565 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C2(H2A,H2B), C1(H1A,H1B), C4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C11(H11), C8(H8)
;
_shelx_res_checksum              66868
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id 92_58-67-Co
_olex2_submission_special_instructions 'No special instructions were received'