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_1565733
_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         'C24 H28 Co N4 O6'
_chemical_formula_sum            'C24 H28 Co N4 O6'
_chemical_formula_weight         527.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 112.724(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.655(7)
_cell_length_b                   10.152(7)
_cell_length_c                   11.788(8)
_cell_measurement_reflns_used    8762
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.50
_cell_measurement_theta_min      2.74
_cell_volume                     1176.1(14)
_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 0.973
_diffrn_measured_fraction_theta_max 0.811
_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  0.2215
_diffrn_reflns_av_unetI/netI     0.3657
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8762
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.783
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.873
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0768 before and 0.0562 after correction. The Ratio of minimum to maximum transmission is 0.7279. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       needle
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.048
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 347 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4227
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.2480
_refine_ls_R_factor_gt           0.1166
_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^)+(0.0953P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.3138
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.751
_reflns_number_gt                1722
_reflns_number_total             4227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           p21
_cod_original_cell_volume        1176.2(14)
_cod_database_code               1565733
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C10)
Uanis(C1) = Uanis(C2) = Uanis(C4) = Uanis(C6)
Uanis(C8) = Uanis(C9) = Uanis(C10)
Uanis(C24) = Uanis(C23) = Uanis(C21) = Uanis(C20) = Uanis(C22)
3.a Riding coordinates:
 N2(H2)
3.b Ternary CH refined with riding coordinates:
 C8(H8)
3.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B)
3.d Aromatic/amide H refined with riding coordinates:
 N3(H3), C11(H11), C12(H12), C13(H13), C15(H15), C20(H20), C22(H22), C23(H23),
 C24(H24)
3.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'