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_7224506
_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 N2 O6, 2(Cl), H2 O'
_chemical_formula_sum            'C24 H34 Cl2 N2 O7'
_chemical_formula_weight         533.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-12
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_audit_update_record
;
2016-02-08 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                   10.6102(10)
_cell_length_b                   21.855(2)
_cell_length_c                   22.183(2)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.108
_cell_measurement_theta_min      2.323
_cell_volume                     5143.9(8)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0877
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.864
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1710 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.8380.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       needle
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11495
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+3.3567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8549
_reflns_number_total             11495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00360e2.cif
_cod_data_source_block           ligand1
_cod_depositor_comments
'Adding full bibliography for 7224504--7224506.cif.'
_cod_database_code               7224506
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.72(9) 0.28(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 H1WA-O1W = O1W-H1WB
 0.995 with sigma of 0.02
 O2W-H2WA
 0.995 with sigma of 0.005
 H2WA-O2W = O2W-H2WB
 0.995 with sigma of 0.02
 H1WA-H1WB
 1.62 with sigma of 0.04
 H2WA-H2WB
 1.62 with sigma of 0.04
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2A), N4(H4A), N3(H3A)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C8(H8A,H8B), C12(H12A,H12B), C14(H14A,H14B),
 C11(H11A,H11B), C6(H6A,H6B), C10(H10A,H10B), C15(H15A,H15B), C9(H9A,H9B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C39(H39A,H39B), C33(H33A,H33B),
  C37(H37A,H37B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C38(H38A,H38B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C23(H23), C24(H24), C17(H17), C18(H18), C4(H4), C21(H21), C22(H22),
 C47(H47), C42(H42), C27(H27), C41(H41), C48(H48), C28(H28), C46(H46), C45(H45)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O7(H7), O11(H11)
;
_shelx_res_checksum              41895
_shelx_shelxl_version_number     2014/7
_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 ligand1
_olex2_submission_special_instructions 'No special instructions were received'