#------------------------------------------------------------------------------
#$Date: 2019-11-03 11:18:32 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221245 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/81/4128115.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4128115
loop_
_publ_author_name
'Du, Kang'
'Thorarinsdottir, Agnes E.'
'Harris, T. David'
_publ_section_title
;
 Selective Binding and Quantitation of Calcium with a Cobalt-Based
 Magnetic Resonance Probe.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7163
_journal_page_last               7172
_journal_paper_doi               10.1021/jacs.9b02661
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '2(C26 H36 Co N4 Na O9), N O3'
_chemical_formula_sum            'C52 H72 Co2 N9 Na2 O21'
_chemical_formula_weight         1323.02
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   34.793(3)
_cell_length_b                   34.793(3)
_cell_length_c                   34.793(3)
_cell_measurement_reflns_used    9143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.85
_cell_measurement_theta_min      2.62
_cell_volume                     42119(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            589157
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         1.434
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             16584
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.320
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7229
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      2.319
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_gt           0.1523
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4727
_refine_ls_wR_factor_ref         0.4885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5967
_reflns_number_total             7229
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b02661_si_003.cif
_cod_data_source_block           LCoNaNO3
_cod_original_cell_volume        42117(11)
_cod_database_code               4128115
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C25-O1
 1.43 with sigma of 0.005
 O1-C1
 1.43 with sigma of 0.005
 C2-O2
 1.43 with sigma of 0.005
 O2-C3
 1.43 with sigma of 0.005
 O3-C4
 1.43 with sigma of 0.005
 O3-C5
 1.43 with sigma of 0.005
 C6-O4
 1.43 with sigma of 0.005
 O4-C7
 1.43 with sigma of 0.005
 C1-C2
 1.54 with sigma of 0.005
 C3-C4
 1.54 with sigma of 0.005
 C5-C6
 1.54 with sigma of 0.005
 O11-H11B
 0.96 with sigma of 0.001
 H11A-H11B
 1.55 with sigma of 0.001
 Na1-H11B
 -3 with sigma of 0.02
 Na1-H11A
 -3 with sigma of 0.02
 O11-H11B \\sim O11-H11A
 with sigma of 0.02
3. Rigid bond restraints
 O1, O2, O3, O4, C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim O2 \\sim C3: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
5.a Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), C4(H4C,H4D), C5(H5A,H5B), C6(H6A,H6B),
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C22(H22), C23(H23), C24(H24)
5.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B)
;
