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_7126305
_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 H14 N2 O3, H2 O'
_chemical_formula_sum            'C11 H16 N2 O4'
_chemical_formula_weight         240.26
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-09
_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                87.473(5)
_cell_angle_beta                 79.192(6)
_cell_angle_gamma                79.227(5)
_cell_formula_units_Z            2
_cell_length_a                   6.8265(12)
_cell_length_b                   7.2475(13)
_cell_length_c                   13.022(2)
_cell_measurement_reflns_used    5616
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      3.09
_cell_volume                     621.65(18)
_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      299.09
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13404
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.090
_diffrn_source                   X-ray
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.151
_exptl_transmission_factor_max   0.983
_exptl_transmission_factor_min   0.978
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2179
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0974P)^2^+0.2375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1696
_reflns_number_total             2179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00943a2.cif
_cod_data_source_block           OMePh-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_original_cell_volume        621.66(18)
_cod_database_code               7126305
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C10A-O3A
 1.25 with sigma of 0.025
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O3)=FVAR(1)
 Sof(N1A)=1-FVAR(2)
 Sof(N1)=FVAR(2)
 Fixed Sof: H1A(0.35) H9AA(0.65) H9AB(0.65) H9AC(0.65) H9BD(0.35) H9BE(0.35)
 H9BF(0.35) N2A(0.65) C10A(0.35) C10B(0.65) N2B(0.35) H1(0.65)
5.a Free rotating group:
 O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), C5(H5), C6(H6), C3(H3), C2(H2)
5.c Idealised Me refined as rotating group:
 C9(H9AA,H9AB,H9AC), C9(H9BD,H9BE,H9BF), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              28829
_olex2_submission_special_instructions 'No special instructions were received'