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_1565736
_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         'C35 H44 Co2 N4 O10, 2(H2 O)'
_chemical_formula_sum            'C35 H48 Co2 N4 O12'
_chemical_formula_weight         834.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90.2670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5972(10)
_cell_length_b                   23.6951(19)
_cell_length_c                   13.4045(11)
_cell_measurement_reflns_used    6950
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      2.36
_cell_volume                     4001.1(6)
_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 0.999
_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  0.0633
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32117
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.375
_diffrn_reflns_theta_min         1.617
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0670 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.8696. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.213
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0904
_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^)+(0.1356P)^2^+13.9410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2578
_refine_ls_wR_factor_ref         0.2907
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4469
_reflns_number_total             7348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5.cif
_cod_data_source_block           p21c
_cod_database_code               1565736
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.737
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N3) = Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29)
Uanis(C11) = Uanis(C5) = Uanis(C3) = Uanis(C2)
Uanis(C13) = Uanis(C22) = Uanis(C16) = Uanis(C21)
3. Others
 Fixed Sof: H2A(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) H5(0.5) C11(0.5)
 H11A(0.5) H11B(0.5) H11C(0.5) H13(0.5) H16(0.5) C21(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 C30(0.5) H30A(0.5) H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5)
 H32B(0.5)
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Ternary CH refined with riding coordinates:
 C2(H2A), C5(H5), C13(H13), C16(H16)
4.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C14(H14A,H14B), C15(H15A,H15B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
4.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C23(H23), C24(H24), C26(H26), C27(H27), C35(H35), C36(H36),
 C38(H38), C39(H39)
4.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'