Hemispherand-Strapped Calix[4]pyrrole: An Ion-pair Receptor for the Recognition and Extraction of Lithium Nitrite.
He, Qing; Zhang, Zhan; Brewster, James T.; Lynch, Vincent M.; Kim, Sung Kuk; Sessler, Jonathan L.; Journal of the American Chemical Society 138 (2016) 9779–9782; doi:10.1021/jacs.6b05713

data_4130669
_publ_section_title
;
 Hemispherand-Strapped Calix[4]pyrrole: An Ion-pair Receptor for the
 Recognition and Extraction of Lithium Nitrite.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9779
_journal_page_last               9782
_journal_paper_doi               10.1021/jacs.6b05713
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C50 H53 Br Li N8 O4, 3(C2 H3 N)'
_chemical_formula_sum            'C56 H65 Br Li N11 O4'
_chemical_formula_weight         1043.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                83.160(2)
_cell_angle_beta                 86.479(2)
_cell_angle_gamma                69.655(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8555(8)
_cell_length_b                   13.8676(8)
_cell_length_c                   14.7764(8)
_cell_measurement_reflns_used    9744
_cell_measurement_temperature    100.1500
_cell_measurement_theta_max      31.1685
_cell_measurement_theta_min      1.3858
_cell_volume                     2642.5(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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
;
????
;
_diffrn_ambient_temperature      100.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
scan:
	Number of images: 268
	           Slice: -110.0000 - 24.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -60.0000
	             Phi: 120.0000
	             XTD: 45.2335
	          2theta: -19.9357
scan:
	Number of images: 268
	           Slice: -110.0000 - 24.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -60.0000
	             Phi: 240.0000
	             XTD: 45.2335
	          2theta: -19.9357
scan:
	Number of images: 268
	           Slice: -110.0000 - 24.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -60.0000
	             Phi: 120.0000
	             XTD: 45.2335
	          2theta: -19.9357
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 45.2335
	          2theta: -19.9357
scan:
	Number of images: 240
	           Slice: -50.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 60.0000
	             Phi: 120.0000
	             XTD: 45.2335
	          2theta: -19.9357
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_method       dtprofit1.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0291
_diffrn_orient_matrix_UB_12      0.0284
_diffrn_orient_matrix_UB_13      0.0651
_diffrn_orient_matrix_UB_21      0.0380
_diffrn_orient_matrix_UB_22      -0.0656
_diffrn_orient_matrix_UB_23      0.0144
_diffrn_orient_matrix_UB_31      0.0542
_diffrn_orient_matrix_UB_32      0.0408
_diffrn_orient_matrix_UB_33      0.0048
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36071
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         9281
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0424
_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/[\s^2^(Fo^2^)+(0.0496P)^2^+3.3926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8240
_reflns_number_total             9281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05713_si_004.cif
_cod_data_source_block           b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'None' was changed
to 'none' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4130669
_diffrn_number_total             317
_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
2. Restrained distances
 O4-H4B
 0.85 with sigma of 0.01
 C50-H4B
 1.89162 with sigma of 0.02
 Li1-H4B
 2.501303 with sigma of 0.02
3. Restrained planarity
 O1, C40, N8, C41
 with sigma of 0.01
 O1A, C40A, N8, C41
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C40 \\sim O1A \\sim C40A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C40) = Uanis(C40A)
5. Same fragment restrains
{O1, C40} sigma for 1-2: 0.01, 1-3: 0.04
as
{O1A, C40A}
6. Others
 Fixed Sof: O1(0.57) C40(0.57) O1A(0.43) C40A(0.43)
7.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C42(H42A,H42B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C13(H13), C14(H14), C18(H18), C19(H19),
 C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37),
  C38(H38), N1(H1), N2(H2), N3(H3A), N4(H4A), N5(H5)
7.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              25110
_shelx_hkl_checksum              61169
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'