Structural diversity in cobalt camphorate coordination polymers with flexible dipyridylamide ligands including looped layers and self-penetrated topologies
Przybyla, Jack J.; Ezenyilimba, Frederick C.; LaDuca, Robert L.; Inorganica Chimica Acta 498 (2019) 119087–; doi:10.1016/j.ica.2019.119087

data_1565735
_publ_section_title
;
 Structural diversity in cobalt camphorate coordination polymers with
 flexible dipyridylamide ligands including looped layers and
 self-penetrated topologies
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119087
_journal_paper_doi               10.1016/j.ica.2019.119087
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C28 H34 Co N4 O6'
_chemical_formula_sum            'C28 H34 Co N4 O6'
_chemical_formula_weight         581.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.518(4)
_cell_length_b                   9.241(2)
_cell_length_c                   15.071(3)
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.52
_cell_measurement_theta_min      2.40
_cell_volume                     2857.6(10)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23350
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.511
_diffrn_reflns_theta_min         1.351
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0766 before and 0.0708 after correction. The Ratio of minimum to maximum transmission is 0.9109. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1033 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5310
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.1025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0916P)^2^+10.7571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2582
_refine_ls_wR_factor_ref         0.2800
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                3552
_reflns_number_total             5310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           p21212
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        2857.7(11)
_cod_database_code               1565735
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. 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 C(H,H,H) groups
2. Restrained distances
 C11A-C10A
 1.55 with sigma of 0.02
 C10-C11
 1.55 with sigma of 0.02
 C9A-C10A
 1.55 with sigma of 0.02
 C10-C9
 1.55 with sigma of 0.02
 C9-C8
 1.55 with sigma of 0.02
 C9A-C8A
 1.55 with sigma of 0.02
 C8A-C7A
 1.55 with sigma of 0.02
 C7-C8
 1.55 with sigma of 0.02
 N3A-C7A
 1.55 with sigma of 0.02
 N3-C7
 1.55 with sigma of 0.02
 N4A-C12A
 1.55 with sigma of 0.02
 N4-C12
 1.55 with sigma of 0.02
 C11A-C12
 1.55 with sigma of 0.02
 C11-C12A
 1.55 with sigma of 0.02
 C30-C29
 1.55 with sigma of 0.02
 C28-C30
 1.55 with sigma of 0.02
 C30-C28
 1.55 with sigma of 0.02
 C21-C20
 1.55 with sigma of 0.02
 C34-C21
 1.55 with sigma of 0.02
 C22-C21
 1.55 with sigma of 0.02
 C24-C20
 1.55 with sigma of 0.02
 C25-C20
 1.55 with sigma of 0.02
 C25-C23
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N4A) = Uanis(N4) = Uanis(C12A) = Uanis(C12) = Uanis(C11) = Uanis(C11A) =
Uanis(C10) = Uanis(C10A) = Uanis(C9A) = Uanis(C8) = Uanis(C8A) = Uanis(C9) =
Uanis(C7A) = Uanis(C7) = Uanis(N3) = Uanis(N3A)
Uanis(C29) = Uanis(C30) = Uanis(C28)
Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C27) = Uanis(C26) = Uanis(C31) =
Uanis(C32) = Uanis(C33) = Uanis(O3) = Uanis(O4)
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C34) = Uanis(C24) =
Uanis(C25) = Uanis(C23)
4. Others
 Fixed Sof: N3(0.5) H3(0.5) N3A(0.5) H3A(0.5) N4(0.5) H4(0.5) N4A(0.5)
 H4A(0.5) C7(0.5) H7A(0.5) H7B(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 C9A(0.5) H9AA(0.5) H9AB(0.5) C10(0.5) H10A(0.5) H10B(0.5) C10A(0.5) H10C(0.5)
 H10D(0.5) C11(0.5) H11A(0.5) H11B(0.5) C11A(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C12A(0.5) H12C(0.5) H12D(0.5) H20(0.5) C21(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C23(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5)
 H25B(0.5) H27(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
5.a Riding coordinates:
 N3A(H3A), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C)
5.b Ternary CH refined with riding coordinates:
 C20(H20), C27(H27)
5.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C7A(H7AA,H7AB), C8(H8A,H8B), C8A(H8AA,H8AB), C9(H9A,H9B),
 C9A(H9AA,H9AB), C10(H10A,H10B), C10A(H10C,H10D), C11(H11A,H11B), C12(H12A,
 H12B), C12A(H12C,H12D), C25(H25A,H25B), C32(H32A,H32B), C33(H33A,H33B)
5.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N4A(H4A), C1(H1), C2(H2), C4(H4B), C5(H5), C14(H14), C15(H15),
  C17(H17), C18(H18)
5.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'