Exploiting the Pyrazole-Carboxylate Mixed Ligand System in the Crystal Engineering of Coordination Polymers
Hawes, Chris S.; Moubaraki, Boujemaa; Murray, Keith S.; Kruger, Paul E.; Turner, David R.; Batten, Stuart R.; Crystal Growth & Design 14 (2014) 5749–; doi:10.1021/cg501004u

data_4512129
_publ_section_title
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 Exploiting the Pyrazole-Carboxylate Mixed Ligand System in the Crystal
 Engineering of Coordination Polymers
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5749
_journal_paper_doi               10.1021/cg501004u
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C62 H60 Co2 N12 O18, H2 O'
_chemical_formula_sum            'C62 H62 Co2 N12 O19'
_chemical_formula_weight         1397.10
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.0516(6)
_cell_length_b                   21.3252(7)
_cell_length_c                   9.1395(3)
_cell_measurement_reflns_used    9083
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.42
_cell_volume                     2933.58(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0635
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            111189
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0798 before and 0.0635 after correction.
The Ratio of minimum to maximum transmission is 0.9500.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.7165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                7533
_reflns_number_total             8630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501004u_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512129--4512135.cif.'
_cod_database_code               4512129
_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) groups, All O(H,H) groups
2. Restrained distances
 H47B-O47
 0.87 with sigma of 0.02
 H47A-H47B
 1.39 with sigma of 0.02
 H48B-O45_$1
 2.44 with sigma of 0.01
 O40_$2-H48A
 3.16 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O48) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O48(0.5) H48A(0.5) H48B(0.5)
5.a Free rotating group:
 O48(H48A,H48B)
5.b Rotating group:
 O47(H47A)
5.c Ternary CH refined with riding coordinates:
 C20(H20), C42(H42)
5.d Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
5.e Aromatic/amide H refined with riding coordinates:
 N3(H3), N13(H13), C30(H30), C31(H31), C38(H38), C39(H39)
5.f Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C21(H21A,H21B,H21C), C43(H43A,H43B,H43C)
;