Conformational control of N-methyl-N,N'-diacylhydrazines by noncovalent carbon bonding in solution.
Deka, Jugal Kishore Rai; Sahariah, Biswajit; Baruah, Kalpita; Bar, Arun Kumar; Sarma, Bani Kanta; Chemical communications (Cambridge, England) 56 (2020) 4874–4877; doi:10.1039/d0cc00943a

data_7126310
_publ_section_title
;
 Conformational control of N-methyl-N,N'-diacylhydrazines by noncovalent
 carbon bonding in solution.
;
_journal_issue                   36
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4874
_journal_page_last               4877
_journal_paper_doi               10.1039/d0cc00943a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C11 H11 F3 N2 O2, H2 O'
_chemical_formula_sum            'C11 H13 F3 N2 O3'
_chemical_formula_weight         278.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-17 deposited with the CCDC.	2020-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.691(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.405(3)
_cell_length_b                   6.5909(10)
_cell_length_c                   14.669(2)
_cell_measurement_reflns_used    2458
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.32
_cell_volume                     1340.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      299.13
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.320
_diffrn_source                   X-ray
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.145
_exptl_transmission_factor_max   0.977
_exptl_transmission_factor_min   0.969
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0782
_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^)+(0.1225P)^2^+1.1649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1275
_reflns_number_total             2364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00943a2.cif
_cod_data_source_block           CF3Ph-NH_NMe-Me
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126305--7126311.cif.
;
_cod_database_code               7126310
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.968
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-H1A
 0.9 with sigma of 0.05
 O1-H1C
 0.95 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(F2A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F3)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uanis(F2) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1A)
\\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F3A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1A)
\\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.9 and
sigma for terminal atoms of 1.8
Uanis(O2B) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N1B) \\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
Uanis(F2B) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F1B) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(F1A) = Uanis(F1) = Uanis(F2A) = Uanis(F2) = Uanis(F3A) = Uanis(F3)
Uanis(O2B) = Uanis(O2A)
Uanis(N1B) = Uanis(N1A)
Uanis(C1B) = Uanis(C1A)
4. Others
 Fixed Sof: O2A(0.5) N1A(0.5) N2A(0.5) F3(0.4) F1(0.4) F2(0.4) F2A(0.4)
 F3A(0.4) F1A(0.4) N2B(0.5) C1A(0.5) C1B(0.5) O2B(0.5) N1B(0.5) F2B(0.2)
 F3B(0.2) F1B(0.2)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              91475
_olex2_submission_special_instructions 'No special instructions were received'